CN1762453A - Essential oil of 'Shiquan Dabu Wan', namely beta-cyclodextrin inclusion compound and its preparation process - Google Patents
Essential oil of 'Shiquan Dabu Wan', namely beta-cyclodextrin inclusion compound and its preparation process Download PDFInfo
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Abstract
The invention relates to a traditional Chinese medicinal medicament containing volatile fluid of general tonic pills and its preparing process, wherein the constituents include (by weight portions): volatile fluid of general tonic pills 1 part, beta-cyclodextrin 3-15 parts, water 20-140 parts.
Description
Technical field
The present invention relates to a kind of tonification class Chinese patent medicine and preparation technology thereof who contains volatile oil, be specifically related to a kind of bolus of ten powerful tonics volatile oil that strengthens bolus of ten powerful tonics volatile oil stability---Benexate Hydrochloride and preparation technology thereof.
Background technology
Bolus of ten powerful tonics is a kind of tonification class Chinese patent medicine of classics, it is to be raw material with Radix Codonopsis, the Rhizoma Atractylodis Macrocephalae, Poria, Radix Glycyrrhizae, Radix Angelicae Sinensis, Rhizoma Chuanxiong, the Radix Paeoniae Alba, Radix Rehmanniae Preparata, the Radix Astragali and Cortex Cinnamomi, preparation in proportion, extract the pharmaceutical preparation that volatile oil is made, cure mainly QI and blood deficiency, pale complexion, the cardiopalmus of breathing hard, dizzy spontaneous perspiration, extremity is not warm.Existing medicinal piece of shiquan dabu pill is volatile because of its volatile oil, and stability of drug is relatively poor, and bioavailability is not high.
Summary of the invention
The object of the present invention is to provide a kind of bolus of ten powerful tonics volatile oil that strengthens bolus of ten powerful tonics volatile oil stability---Benexate Hydrochloride and preparation technology thereof.
The technical scheme that realizes above-mentioned purpose is: bolus of ten powerful tonics volatile oil is carried out beta-cyclodextrin inclusion compound get clathrate, this bolus of ten powerful tonics volatile oil---Benexate Hydrochloride, it is by bolus of ten powerful tonics volatile oil, beta-schardinger dextrin-and water are formed, the parts by weight of each component are: 1 part of bolus of ten powerful tonics volatile oil, 3～15 parts of beta-schardinger dextrin-s, 20～140 parts in water, described component is through stirring, cooling, the centrifugal precipitate that gets, drying forms beta-cyclodextrin inclusion compound bolus of ten powerful tonics volatile oil, wherein said bolus of ten powerful tonics volatile oil is to be 60～100 parts of the Rhizoma Atractylodis Macrocephalaes by weight, 100～140 parts of Radix Angelicae Sinensis, 10～30 parts of 20～60 parts of Rhizoma Chuanxiongs and Cortex Cinnamomis add water and carry out steam distillation and extract and obtain.
Described bolus of ten powerful tonics volatile oil---the preparation technology of Benexate Hydrochloride comprises the steps:
1). get raw material by weight: 1 part of bolus of ten powerful tonics volatile oil, 3～12 parts of beta-schardinger dextrin-s, 20～140 parts in water, wherein bolus of ten powerful tonics volatile oil is to be 10～30 parts of 60～100 parts of the Rhizoma Atractylodis Macrocephalaes, 100～140 parts of Radix Angelicae Sinensis, 20～60 parts of Rhizoma Chuanxiongs and Cortex Cinnamomis by weight, adds water and carries out steam distillation and extract and obtain;
2). beta-schardinger dextrin-is mixed with water, be heated to 50～70 ℃ of dissolvings, be chilled to 25 ± 10 ℃ and make the beta-schardinger dextrin-aqueous solution;
3). in the beta-schardinger dextrin-aqueous solution that step 2 makes, add bolus of ten powerful tonics volatile oil, with agitator or organize broken machine to stir, mixing time is 5-120 minute, place down at＜5 ℃, the centrifugal precipitate that gets, dry 1～3d promptly gets bolus of ten powerful tonics volatile oil---Benexate Hydrochloride under＜60 ℃ of room temperature.
Bolus of ten powerful tonics volatile oil of the present invention---Benexate Hydrochloride is used to prepare the various preparations of bolus of ten powerful tonics
1), the preparation of granule,
Get 60～100 parts of 60～100 parts of Radix Codonopsis, 60～100 parts in Poria, 20～60 parts in Radix Glycyrrhizae, 60～100 parts of the Radix Paeoniae Albas, 100～140 parts of Radix Rehmanniae Preparata and the Radixs Astragali by weight, adding water is 10～15 times of decoction secondaries of described Six-element medical material gross weight, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate is left standstill; Get 10～30 parts of 60～100 parts of the supernatant and the Rhizoma Atractylodis Macrocephalaes, 100～140 parts of Radix Angelicae Sinensis, 20～60 parts of Rhizoma Chuanxiongs and Cortex Cinnamomis add water carry out steam distillation extract residual liquid behind the volatile oil and medicinal residues filter aqueous solution merge, be concentrated into 1～2 times of above-mentioned ten flavor medical material weight, add ethanol equivalent and make precipitation; Get supernatant concentration and become thick paste, add cane sugar powder, thick paste and cane sugar powder are 1: 1～6 by weight, make particulate matter, dry under＜80 ℃ of room temperature, put coldly, add volatile oil---the Benexate Hydrochloride of the volatile oil preparation that the above-mentioned Rhizoma Atractylodis Macrocephalae, Radix Angelicae Sinensis, Rhizoma Chuanxiong and Cortex Cinnamomi extract, mixing promptly gets granule.
2), the preparation of tablet,
Get 60～100 parts of Radix Codonopsis, 60～100 parts in Poria, 20～60 parts in Radix Glycyrrhizae, 60～100 parts of the Radix Paeoniae Albas, 100～140 parts of Radix Rehmanniae Preparata and 60～100 parts of the Radixs Astragali by weight, add 10～15 times of decoction secondaries that water is described Six-element medical material gross weight, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate is left standstill; Get 60～100 parts of the supernatant and the Rhizoma Atractylodis Macrocephalaes, 100～140 parts of Radix Angelicae Sinensis, 10～30 parts of 20～60 parts of Rhizoma Chuanxiongs and Cortex Cinnamomis add water carry out steam distillation extract residual liquid behind the volatile oil and medicinal residues filter aqueous solution merge, be concentrated into 1～2 times of above-mentioned ten flavor medical material weight, add ethanol equivalent and make precipitation, get supernatant concentration and become thick paste, add cane sugar powder, thick paste and cane sugar powder are 1: 1～6 by weight, make particulate matter, dry under＜80 ℃ of room temperature, put coldly, add the above-mentioned Rhizoma Atractylodis Macrocephalae, Radix Angelicae Sinensis, volatile oil---the Benexate Hydrochloride of the volatile oil preparation that Rhizoma Chuanxiong and Cortex Cinnamomi are extracted, tabletting, coating promptly gets tablet.
3), the preparation of capsule,
Get 60～100 parts of Radix Codonopsis, 60～100 parts in Poria, 20～60 parts in Radix Glycyrrhizae, 60～100 parts of the Radix Paeoniae Albas, 100～140 parts of Radix Rehmanniae Preparata and 60～100 parts of the Radixs Astragali by weight, add 10～15 times of decoction secondaries that water is described Six-element medical material gross weight, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate is left standstill; Get 60～100 parts of the supernatant and the Rhizoma Atractylodis Macrocephalaes, 100～140 parts of Radix Angelicae Sinensis, 10～30 parts of 20～60 parts of Rhizoma Chuanxiongs and Cortex Cinnamomis add water carry out steam distillation extract residual liquid behind the volatile oil and medicinal residues filter aqueous solution merge, be concentrated into 1～2 times of above-mentioned ten flavor medical material weight, add ethanol equivalent and make precipitation, get supernatant concentration and become thick paste, add cane sugar powder, thick paste and cane sugar powder are 1: 1～6 by weight, make particulate matter, dry under＜80 ℃ of room temperature, put coldly, add the above-mentioned Rhizoma Atractylodis Macrocephalae, Radix Angelicae Sinensis, volatile oil---the Benexate Hydrochloride of the volatile oil preparation that Rhizoma Chuanxiong and Cortex Cinnamomi are extracted, mixing, the capsulae vacuus of packing into promptly gets capsule.
Cyclodextrin inclusion technique is meant that a kind of molecule is embedded in by bag in the opening structure of another kind of molecule, forms the technology of clathrate.This clathrate is to be formed by host molecule and two kinds of component adductions of enclosed molecule, and host molecule has bigger opening structure, in being enough to enclosed molecule is contained in.Clathrate behind the enclose can improve significantly by many physicochemical properties such as the dissolubility of enclose medicine, stability.The present invention can prevent the bolus of ten powerful tonics volatile oils by beta-cyclodextrin inclusion compound bolus of ten powerful tonics volatile oil, strengthen the stability of bolus of ten powerful tonics volatile oil, increase its water solublity, improve its bioavailability, provide reliable assurance for further developing bolus of ten powerful tonics series oral formulations.
Mixture to beta-schardinger dextrin-and bolus of ten powerful tonics volatile oil, the clathrate of beta-schardinger dextrin-and bolus of ten powerful tonics volatile oil is tested respectively, the result shows, the X-diffraction pattern of Benexate Hydrochloride has than big-difference bolus of ten powerful tonics volatile oil---beta-schardinger dextrin-mixture and bolus of ten powerful tonics volatile oil---, mixture is the stack at volatile oil and beta-schardinger dextrin-diffractive features peak, and clathrate shows brand-new collection of illustrative plates. (seeing Fig. 1-3).
Stability experiment shows, the stability of bolus of ten powerful tonics volatile oil---Benexate Hydrochloride better, prediction effect duration reaches 2 years, meets the regulation that medicine is deposited.
Description of drawings
Fig. 1 is the X-ray diffracting spectrum of bolus of ten powerful tonics volatile oil and beta-schardinger dextrin-mixture
Fig. 2 is the X-ray diffracting spectrum of beta-schardinger dextrin-
Fig. 3 is bolus of ten powerful tonics volatile oil of the present invention---the X-ray diffracting spectrum of Benexate Hydrochloride
Fig. 4 is the infrared comparison diagram of beta-schardinger dextrin-, Benexate Hydrochloride
Fig. 1-3X-ray diffraction method test condition:
D/MAX-IIIA type x x ray diffractometer x (Japanese Rikagu of science); Scan mode: qualitative, step-scan; Voltage/current: 35kV/30mA; Scanning speed: 10 °/min; Step-length: 0.02 ° (2 θ); Preset time: 0.2s; Target: Cu target; Sweep limits: (2 θ) 5-60 °.
By Fig. 1-3 as can be known, beta-schardinger dextrin-, both mixture, both clathrate are tested respectively, the result shows, the X-diffraction pattern of bolus of ten powerful tonics volatile oil beta-cyclodextrin mixture and bolus of ten powerful tonics volatile oil beta cyclodextrin inclusion complex has than big-difference, mixture is the stack at volatile oil and beta-schardinger dextrin-diffractive features peak, and clathrate shows brand-new collection of illustrative plates, thereby judges the enclose success.
The infared spectrum method of testing of Fig. 4
WQF-200 type Fourier transformation infrared spectrometer: (second optical instrument factory, Beijing)
Take by weighing about 200mg potassium bromide, in agate mortar, be ground into fine powder, dry in drying baker.Take by weighing the about 2mg of beta-schardinger dextrin-again, place agate mortar, add dry good potassium bromide, grind mixing, tabletting in compression mold, visual detection, slice, thin piece is transparence.The slice, thin piece of gained is detected in Fourier infrared spectrograph, obtain collection of illustrative plates.See 1 among Fig. 4.
Get the clathrate kbr tablet according to last legal system, the slice, thin piece of gained is detected in Fourier infrared spectrograph, obtain collection of illustrative plates.See 2 among Fig. 4.
As shown in Figure 4, at finger print region, the trap at the peak of clathrate is higher than the trap at the peak of beta-schardinger dextrin-, the former peak than the latter's peak a little less than and short, and all move to the long wave direction position at peak, peak in some beta-schardinger dextrin-disappears in inclusion complex, and above phenomenon also illustrates that volatile oil is by the beta-schardinger dextrin-inclusion.
The specific embodiment
The bolus of ten powerful tonics prescription is a prior art, and the weight portion proportioning is 10～30 parts of 60～100 parts of Radix Codonopsis, 60～100 parts of the Rhizoma Atractylodis Macrocephalaes, 60～100 parts in Poria, 20～60 parts in Radix Glycyrrhizae, 100～140 parts of Radix Angelicae Sinensis, 20～60 parts of Rhizoma Chuanxiongs, 60～100 parts of the Radix Paeoniae Albas, 100～140 parts of Radix Rehmanniae Preparata, 60～100 parts of the Radixs Astragali and Cortex Cinnamomis.Optimum weight part proportioning is: 20 parts of 80 parts of Radix Codonopsis, 80 parts of the Rhizoma Atractylodis Macrocephalaes, 80 parts in Poria, 40 parts in Radix Glycyrrhizae, 120 parts of Radix Angelicae Sinensis, 40 parts of Rhizoma Chuanxiongs, 80 parts of the Radix Paeoniae Albas, 120 parts of Radix Rehmanniae Preparata, 80 parts of the Radixs Astragali and Cortex Cinnamomis.
It is prior art that bolus of ten powerful tonics extracts volatile oil: choose 10～30 parts of 60～100 parts of the Rhizoma Atractylodis Macrocephalaes, 100～140 parts of Radix Angelicae Sinensis, 20～60 parts of Rhizoma Chuanxiongs and Cortex Cinnamomis by weight, adding water carries out steam distillation and extracts and to obtain volatile oil, aqueous solution and medicinal residues filter, the medicinal residues water continues to decoct 1 hour, filter, merge twice filtrate and promptly get the solution for standby of extracting behind the volatile oil.
The used beta-schardinger dextrin-of the present invention (β-CD): purity 〉=95%; Used instrument also has: magnetic stirring apparatus; DS-1 high-speed tissue mashing machine; Volatile oil determination apparatud; The illumination experiment instrument;
Embodiment 1:
Bolus of ten powerful tonics volatile oil-Benexate Hydrochloride, it is made up of bolus of ten powerful tonics volatile oil, beta-schardinger dextrin-and water, and the parts by weight of each component are: 1 part of bolus of ten powerful tonics volatile oil, 3 parts of beta-schardinger dextrin-s, 20 parts in water.
The preparation technology of above-mentioned bolus of ten powerful tonics volatile oil-Benexate Hydrochloride comprises the steps: 1). be by weight: 1 part of bolus of ten powerful tonics volatile oil, β-3 parts of ring pastes, water are chosen raw material for 20 parts; 2). beta-schardinger dextrin-is mixed with water, be heated to 50 ℃ of dissolvings, be chilled to 25 ± 5 ℃ and make the beta-schardinger dextrin-aqueous solution; 3). with adding bolus of ten powerful tonics volatile oil in the above-mentioned beta-schardinger dextrin-aqueous solution, stir with agitator, mixing time is 5 minutes, place down at＜5 ℃, the centrifugal precipitate that gets, drying is 1 hour under＜60 ℃ of room temperature, promptly gets bolus of ten powerful tonics volatile oil-Benexate Hydrochloride.
Above-mentioned bolus of ten powerful tonics volatile oil-Benexate Hydrochloride is prepared into granule, tablet or capsule:
Get Radix Codonopsis, Poria, Radix Glycyrrhizae, the Radix Paeoniae Alba, Radix Rehmanniae Preparata and Radix Astragali Six-element, be by weight: 60 parts of Radix Codonopsis, 60 parts in Poria, 20 parts in Radix Glycyrrhizae, 60 parts of the Radix Paeoniae Albas, 100 parts of Radix Rehmanniae Preparata and 60 parts of the Radixs Astragali, water are 10 times of Six-element medical material gross weight, decoct with water secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction filters, and filtrate is left standstill; The aqueous solution of getting behind 80 parts of the supernatant and the weight Rhizoma Atractylodis Macrocephalaes, 120 parts of Radix Angelicae Sinensis, 40 parts of Rhizoma Chuanxiongs and 20 parts of distillating extracting oils of Cortex Cinnamomi merges, be concentrated into 1～2 times of above-mentioned ten flavor medical material weight, add ethanol equivalent and make precipitation, get supernatant concentration and become thick paste, add cane sugar powder, thick paste and cane sugar powder are 1: 1～6 by weight, make particulate matter, dry, put cold, adding makes bolus of ten powerful tonics volatile oil---Benexate Hydrochloride for 20 parts with 80 parts of the weight Rhizoma Atractylodis Macrocephalaes, 120 parts of Radix Angelicae Sinensis, 40 parts of Rhizoma Chuanxiongs and Cortex Cinnamomi, promptly gets granule.Become thick paste if get supernatant concentration, add starch, thick paste and starch are 1: 0.2～2 by weight, make particulate matter, drying, put cold, add bolus of ten powerful tonics volatile oil---the Benexate Hydrochloride that the above-mentioned amount Rhizoma Atractylodis Macrocephalae, Radix Angelicae Sinensis, Rhizoma Chuanxiong and Cortex Cinnamomi make, mixing gets granule, the capsulae vacuus of packing into promptly gets capsule; Continue tabletting if adopt behind the mixing, coating promptly gets tablet.
Embodiment 2:
Bolus of ten powerful tonics volatile oil---Benexate Hydrochloride, it is made up of bolus of ten powerful tonics volatile oil, beta-schardinger dextrin-and water, and the parts by weight of each component are: 1 part of bolus of ten powerful tonics volatile oil, 15 parts of beta-schardinger dextrin-s, 140 parts in water.
The preparation technology of above-mentioned bolus of ten powerful tonics volatile oil-Benexate Hydrochloride comprises the steps: 1). choose raw material: be by weight: 1 part of bolus of ten powerful tonics volatile oil, β-15 parts of ring pastes, 140 parts in water, choose raw material; 2). beta-schardinger dextrin-is mixed with water, be heated to 80 ℃ of dissolvings, be chilled to 25 ± 5 ℃ and make the beta-schardinger dextrin-aqueous solution; 3). with adding bolus of ten powerful tonics volatile oil in the above-mentioned beta-schardinger dextrin-aqueous solution, stir with tissue mashing machine, mixing time is 120 minutes, place down at＜5 ℃, the centrifugal precipitate that gets, drying is 3 hours under＜60 ℃ of room temperature room temperature, promptly gets bolus of ten powerful tonics volatile oil-Benexate Hydrochloride.Wherein extract medical material that bolus of ten powerful tonics volatile oil uses and consumption with embodiment 1.
Embodiment 3:
Bolus of ten powerful tonics volatile oil-Benexate Hydrochloride, it is made up of bolus of ten powerful tonics volatile oil, beta-schardinger dextrin-and water, and the parts by weight of each component are: 1 part of bolus of ten powerful tonics volatile oil, 4 parts of beta-schardinger dextrin-s, 70 parts in water.
The preparation technology of above-mentioned bolus of ten powerful tonics volatile oil-Benexate Hydrochloride comprises the steps: 1). choose raw material: be by weight: 1 part of bolus of ten powerful tonics volatile oil, β-4 parts of ring pastes, 70 parts in water, choose raw material; 2). beta-schardinger dextrin-is mixed with water, be heated to 60 ℃ of dissolvings, be chilled to 25 ± 5 ℃ and make the beta-schardinger dextrin-aqueous solution; 3). with adding bolus of ten powerful tonics volatile oil in the above-mentioned beta-schardinger dextrin-aqueous solution, stir with agitator, mixing time is 60 minutes, place down at＜5 ℃, the centrifugal precipitate that gets, drying is 2 hours under＜60 ℃ of room temperature, promptly gets bolus of ten powerful tonics volatile oil-Benexate Hydrochloride.Wherein extract medical material that bolus of ten powerful tonics volatile oil uses and consumption with embodiment 1
Embodiment 4:
Bolus of ten powerful tonics volatile oil-Benexate Hydrochloride, it is made up of bolus of ten powerful tonics volatile oil, beta-schardinger dextrin-and water, and the parts by weight of each component are: 1 part of bolus of ten powerful tonics volatile oil, 8 parts of beta-schardinger dextrin-s, 100 parts in water.
The preparation technology of above-mentioned bolus of ten powerful tonics volatile oil-Benexate Hydrochloride comprises the steps: 1). choose raw material: be by weight: 1 part of bolus of ten powerful tonics volatile oil, β-8 parts of ring pastes, 100 parts in water, choose raw material; 2). beta-schardinger dextrin-is mixed with water, be heated to 65 ℃ of dissolvings, be chilled to 25 ± 5 ℃ and make the beta-schardinger dextrin-aqueous solution; 3). with adding bolus of ten powerful tonics volatile oil in the above-mentioned beta-schardinger dextrin-aqueous solution, stir with tissue mashing machine, mixing time is 80 minutes, place down at＜5 ℃, the centrifugal precipitate that gets, drying is 2 hours under＜60 ℃ of room temperature, promptly gets bolus of ten powerful tonics volatile oil-Benexate Hydrochloride.Wherein extract medical material that bolus of ten powerful tonics volatile oil uses and consumption with embodiment 1
Embodiment 5:
Bolus of ten powerful tonics volatile oil beta-CD inclusion preparation technology investigates
Adopt saturated water solution method, take by weighing β-CD, add water with the 10ml/g ratio, heating for dissolving is chilled to 25 ± ℃ room temperature.Add bolus of ten powerful tonics volatile oil, with magnetic stirring apparatus or organize broken machine to stir, take out and put into but 1d of refrigerator and cooled.Centrifugal, dry 2d under＜60 ℃ of room temperature promptly gets bolus of ten powerful tonics volatile oil-Benexate Hydrochloride, and different alr modes and mixing time experimental result are listed in table 1, and by table 1 as seen, the proper extension mixing time can increase the yield of clathrate.
Embodiment 6: the light durability experiment of bolus of ten powerful tonics volatile oil-Benexate Hydrochloride
Place lighting box (3000lX) to place 10d bolus of ten powerful tonics volatile oil-beta-CD inclusion, respectively at 0,3,5,10d sampling and measure the bolus of ten powerful tonics volatile oil content with volatile oil determination apparatud, experimental result is listed in table 2.The result shows that the clathrate capsule is stable to light.
Embodiment 7: the high-temperature stability experiment of bolus of ten powerful tonics volatile oil-Benexate Hydrochloride
Experimental result is listed in table 3.As seen from table, temperature is high more, and cosmetic variation is big more.This illustrates that each sample is inner in high temperature experiment complicated variation has taken place, but is not simple zero level or first order reaction, therefore, should method routinely ask and calculates effect duration.
Embodiment 8: bolus of ten powerful tonics volatile oil-Benexate Hydrochloride accelerated tests
Experimental result is listed in table 4.The result shows, the clathrate capsule is at 40 ℃, deposit 3 months under relative humidity 75% condition after, its relative amount is still more than 90%.Press the U.S. FDA standard, the clathrate effect duration with above-mentioned experimental result is more than 2 years.FDA regulation: solid drugs is under 37 ℃～40 ℃, relative humidity 75% or higher situation, and still in prescribed limit, then effect duration is more than 2 years to its effective ingredient.Provide reliable assurance for further developing bolus of ten powerful tonics series oral formulations.
The preparation technology of table 1 bolus of ten powerful tonics volatile oil clathrate compound investigates the result
| Numbering | β -CD (g) | Bolus of ten powerful tonics volatile oil (mL) | Mixing time (min) | Clathrate output (g) | Clathrate yield (%) | Oil content (%) | Oil utilization rate (%) |
| 1 2 3 4 5 6 | 10.0 10.0 10.0 10.0 10.0 10.0 | 1 1 1 1 2 2 | Stirring 60 stirs 60 and stirs 90 and stir 90 groups 10 groups 10 | 8.83 8.63 9.29 9.74 10.6 10.6 | 79.5 77.7 83.7 8.77 95.5 88.8 | 7.97 7.77 9.35 8.47 7.89 8.41 | 64 61 79 75 76 81 |
Table 2 bolus of ten powerful tonics volatile oil clathrate compound illumination experimental result
| Time (d) | Outward appearance | Bolus of ten powerful tonics volatile oil abnormal smells from the patient | Clathrate oil content (%) | Catabolite | Concentration (%) |
| 0 | Little Huang | Little have | 9.35 | Do not have | 100.00 |
| 3 5 10 | The little Huang of the little Huang of little Huang | Little have little have littlely have | 9.31 9.28 9.26 | Do not have | 99.57 99.25 99.03 |
Table 3 bolus of ten powerful tonics volatile oil clathrate compound high temperature experimental result
| Time (d) | Outward appearance | Bolus of ten powerful tonics volatile oil abnormal smells from the patient | Clathrate oil content (%) | Catabolite | Concentration (%) |
| 0 40 | The white little Huang of light yellow complexion of white white white white white is deep yellow | Little have little have little have little have little have little have little have little have little have littlely have | 9.35 9.30 9.23 9.12 8.98 8.91 8.78 9.18 9.01 8.65 | Do not have | 100.00 99.68 98.72 97.54 96.04 95.29 93.90 98.18 96.36 92.51 |
The accelerated tests result of table 4 bolus of ten powerful tonics volatile oil clathrate compound
| Time (d) | Outward appearance | Bolus of ten powerful tonics volatile oil abnormal smells from the patient | Clathrate oil content (%) | Catabolite | Concentration (%) |
| 1 2 3 | The little Huang of the little Huang of little Huang | Little have little have littlely have | 9.14 8.79 8.54 | Do not have | 97.75 94.01 91.34 |
Claims (5)
1. bolus of ten powerful tonics volatile oil---Benexate Hydrochloride, it is characterized in that: it is by bolus of ten powerful tonics volatile oil, beta-schardinger dextrin-and water are formed, the parts by weight of each component are: 1 part of bolus of ten powerful tonics volatile oil, 3～15 parts of beta-schardinger dextrin-s, 20～140 parts in water, described component is through stirring, cooling, the centrifugal precipitate that gets, drying forms beta-cyclodextrin inclusion compound bolus of ten powerful tonics volatile oil, wherein said bolus of ten powerful tonics volatile oil is to be 60～100 parts of the Rhizoma Atractylodis Macrocephalaes by weight, 100～140 parts of Radix Angelicae Sinensis, 10～30 parts of 20～60 parts of Rhizoma Chuanxiongs and Cortex Cinnamomis add water and carry out steam distillation and extract and obtain.
2. the described bolus of ten powerful tonics volatile oil of claim 1---the preparation technology of Benexate Hydrochloride is characterized in that comprising the steps:
1). get raw material by weight: 1 part of bolus of ten powerful tonics volatile oil, 3～12 parts of beta-schardinger dextrin-s, 20～140 parts in water, wherein bolus of ten powerful tonics volatile oil is to be 10～30 parts of 60～100 parts of the Rhizoma Atractylodis Macrocephalaes, 100～140 parts of Radix Angelicae Sinensis, 20～60 parts of Rhizoma Chuanxiongs and Cortex Cinnamomis by weight, adds water and carries out steam distillation and extract and obtain;
2). beta-schardinger dextrin-is mixed with water, be heated to 50～70 ℃ of dissolvings, be chilled to 25 ± 10 ℃ and make the beta-schardinger dextrin-aqueous solution;
3). in the beta-schardinger dextrin-aqueous solution that step 2 makes, add bolus of ten powerful tonics volatile oil, with agitator or organize broken machine to stir, mixing time is 5-120 minute, place down at＜5 ℃, the centrifugal precipitate that gets, dry 1～3d promptly gets bolus of ten powerful tonics volatile oil---Benexate Hydrochloride under＜60 ℃ of room temperature.
3, the described bolus of ten powerful tonics volatile oil of claim 1---Benexate Hydrochloride is used to prepare the bolus of ten powerful tonics granule, it is characterized in that, get 60～100 parts of 60～100 parts of Radix Codonopsis, 60～100 parts in Poria, 20～60 parts in Radix Glycyrrhizae, 60～100 parts of the Radix Paeoniae Albas, 100～140 parts of Radix Rehmanniae Preparata and the Radixs Astragali by weight, adding water is 10～15 times of decoction secondaries of described Six-element medical material gross weight, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate is left standstill; Get 10～30 parts of 60～100 parts of the supernatant and the Rhizoma Atractylodis Macrocephalaes, 100～140 parts of Radix Angelicae Sinensis, 20～60 parts of Rhizoma Chuanxiongs and Cortex Cinnamomis add water carry out steam distillation extract residual liquid behind the volatile oil and medicinal residues filter aqueous solution merge, be concentrated into 1～2 times of above-mentioned ten flavor medical material weight, add ethanol equivalent and make precipitation; Get supernatant concentration and become thick paste, add cane sugar powder, thick paste and cane sugar powder are 1: 1～6 by weight, make particulate matter, dry under＜80 ℃ of room temperature, put coldly, add volatile oil---the Benexate Hydrochloride of the volatile oil preparation that the above-mentioned Rhizoma Atractylodis Macrocephalae, Radix Angelicae Sinensis, Rhizoma Chuanxiong and Cortex Cinnamomi extract, mixing promptly gets granule.
4, the described bolus of ten powerful tonics volatile oil of claim 1---Benexate Hydrochloride is used to prepare the bolus of ten powerful tonics tablet, it is characterized in that getting by weight 60～100 parts of 60～100 parts of Radix Codonopsis, 60～100 parts in Poria, 20～60 parts in Radix Glycyrrhizae, 60～100 parts of the Radix Paeoniae Albas, 100～140 parts of Radix Rehmanniae Preparata and the Radixs Astragali, adding water is 10～15 times of decoction secondaries of described Six-element medical material gross weight, 2 hours for the first time, 1 hour for the second time, collecting decoction filters, and filtrate is left standstill; Get 60～100 parts of the supernatant and the Rhizoma Atractylodis Macrocephalaes, 100～140 parts of Radix Angelicae Sinensis, 20～60 parts of Rhizoma Chuanxiongs conciliate 10～30 parts of Cortex Cinnamomis add water carry out steam distillation extract residual liquid behind the volatile oil and medicinal residues filter aqueous solution merge, be concentrated into 1～2 times of above-mentioned ten flavor medical material weight, add ethanol equivalent and make precipitation, get supernatant concentration and become thick paste, add cane sugar powder, thick paste and cane sugar powder are 1: 1～6 by weight, make particulate matter, dry under＜80 ℃ of room temperature, put coldly, add the above-mentioned Rhizoma Atractylodis Macrocephalae, Radix Angelicae Sinensis, volatile oil---the Benexate Hydrochloride of the volatile oil preparation that Rhizoma Chuanxiong and Cortex Cinnamomi are extracted, tabletting, coating promptly gets tablet.
5, the described bolus of ten powerful tonics volatile oil of claim 1---Benexate Hydrochloride is used to prepare the bolus of ten powerful tonics capsule, it is characterized in that, get 60～100 parts of 60～100 parts of Radix Codonopsis, 60～100 parts in Poria, 20～60 parts in Radix Glycyrrhizae, 60～100 parts of the Radix Paeoniae Albas, 100～140 parts of Radix Rehmanniae Preparata and the Radixs Astragali by weight, adding water is 10～15 times of decoction secondaries of described Six-element medical material gross weight, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate is left standstill; Get 60～100 parts of the supernatant and the Rhizoma Atractylodis Macrocephalaes, 100～140 parts of Radix Angelicae Sinensis, 10～30 parts of 20～60 parts of Rhizoma Chuanxiongs and Cortex Cinnamomis add water carry out steam distillation extract residual liquid behind the volatile oil and medicinal residues filter aqueous solution merge, be concentrated into 1～2 times of above-mentioned ten flavor medical material weight, add ethanol equivalent and make precipitation, get supernatant concentration and become thick paste, add cane sugar powder, thick paste and cane sugar powder are 1: 1～6 by weight, make particulate matter,＜80 ℃ of room temperature are dry down, put coldly, add the above-mentioned Rhizoma Atractylodis Macrocephalae, Radix Angelicae Sinensis, volatile oil---the Benexate Hydrochloride of the volatile oil preparation that Rhizoma Chuanxiong and Cortex Cinnamomi are extracted, mixing, the capsulae vacuus of packing into promptly gets capsule.
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|---|---|---|---|
| CNB2005100195180A CN100391498C (en) | 2005-09-29 | 2005-09-29 | Essential oil of 'Shiquan Dabu Wan', namely beta-cyclodextrin inclusion compound and its preparation process |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100195180A CN100391498C (en) | 2005-09-29 | 2005-09-29 | Essential oil of 'Shiquan Dabu Wan', namely beta-cyclodextrin inclusion compound and its preparation process |
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| CN100391498C CN100391498C (en) | 2008-06-04 |
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