CN102552442B - Compound traditional Chinese medicinal dripping pills for treating hyperosteogeny and preparation method thereof - Google Patents
Compound traditional Chinese medicinal dripping pills for treating hyperosteogeny and preparation method thereof Download PDFInfo
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Abstract
The invention relates to compound traditional Chinese medicinal dripping pills for treating hyperosteogeny, which are prepared by the following steps: proportionally weighing medicinal materials Radix Aconite (processed), aconite roots (processed), Chinese cinnamon, Radix codonopsitis, Angelica sinensis, white peony roots (parched), Herba Epimedii and olibanum (processed), extracting with water for three times, merging supernatants, centrifuging, precipitating with alcohol, and purifying with macroporous adsorption resin to obtain an extract; mixing the extract with a matrix which is a mixture of PEG (polyethylene glycol) 4000 and PEG6000, and dripping with dimethyl silicon oil as a coolant under a certain dripping temperature, dripping aperture, dripping speed and dripping distance to obtain the compound dripping pills. The invention also discloses a preparation method of the compound dripping pills. The traditional Chinese medicinal dripping pills for treating hyperosteogeny, disclosed by the invention, have simple and feasible preparation method and no contamination; and the prepared dripping pills are convenient for administration, have good safety, low adverse side effects and low cost, and are suitable for large-scale production. The dripping pills of the invention have the effects of warming yang, dispelling cold, supplementing qi, activating blood circulation and relieving swelling and pain, and can be used for treating hypertrophic arthritis in cervical vertebrae and knee joints due to insufficiency of yang and cold dampness.
Description
Technical field
The invention belongs to field of traditional Chinese medicine pharmacy, specifically, relate to a kind of compound traditional Chinese medicinal dripping pills for the treatment of hyperosteogeny and preparation method thereof.
Background technology
Treatment hyperosteogeny Chinese medicine compound (former prescription fugui ostealgia compound) is by 13～16 parts of Radix Aconiti Lateralis Preparatas (system), 5～8 parts of Radix Aconitis (system), 2～4 parts of Cortex Cinnamomis, 9～11 parts of Radix Codonopsis, 9～12 parts of Radix Angelicae Sinensis, 9～11 parts of the Radix Paeoniae Albas (stir-fry), 5～8 part of 8 flavor Chinese medicine of 9～11 parts of Herba Epimedii and Olibanum (system) forms, this prescription is got << Jin Kui outline " elite of Aconiti Decoction, be used for the treatment of yang deficiency cold-dampness type cervical vertebra and gonarthrosis, clinical effective rate reaches more than 90%, for treatment yang deficiency cold-dampness type rheumatism, one line medication of the illness such as joint hyperplasia arthritis, in treatment rheumatism, significant role is being brought into play in joint hyperplasia arthritis aspect.The dosage form of current clinical use is mainly: fugui gutong keli agent, fugui ostealgia capsule and FUGUI GUTONG PIAN, dosage form dullness.Above dosage form dissolution rate is slow, absorbs poorly, has different shortcoming and defect separately in clinical practice.
Summary of the invention
The object of the present invention is to provide a kind of method simple, with low cost, be suitable for drop pill of large-scale production, quality controllable treatment hyperosteogeny and preparation method thereof.
For achieving the above object, the present invention takes following technical scheme:
A kind of compound traditional Chinese medicinal dripping pills for the treatment of hyperosteogeny, it is to take ingredients according to 5～8 parts of 13～16 parts of Radix Aconiti Lateralis Preparatas (system), 5～8 parts of Radix Aconitis (system), 2～4 parts of Cortex Cinnamomis, 9～12 parts of Radix Codonopsis, 9～12 parts of Radix Angelicae Sinensis, 9～12 parts of the Radix Paeoniae Albas (stir-fry), 9～12 parts of Herba Epimedii, Olibanum (system), pulverize, cross 10～20 mesh sieves, extract and adjuvant Polyethylene Glycol PEG4000, the Polyethylene Glycol PEG6000 of above-mentioned medical material gained after extracting purification, or the drop pill that is mixed according to 1: 1～4 weight ratio of the mixture of Polyethylene Glycol PEG4000 and Polyethylene Glycol PEG6000.
Drop pill as above, wherein each medical material ratio is: Radix Aconiti Lateralis Preparata (system) 14.8g, Radix Aconiti (system) 7.4g, Radix Codonopsis 11.1g, Radix Angelicae Sinensis 11.1g, Radix Paeoniae Alba 11.1g, Herba Epimedii 11.1g, Olibanum 7.4g, Cortex Cinnamomi 3.7g, take ingredients, pulverize, cross 10～20 mesh sieves.
Drop pill as above, wherein, after said extracted thing purification, with the weight ratio of the mixture of adjuvant Polyethylene Glycol PEG4000 and Polyethylene Glycol PEG6000, be preferably 1: 2～4.
A kind of preparation method for the treatment of the compound traditional Chinese medicinal dripping pills of hyperosteogeny, it is to complete according to the following steps:
A. take following medicinal materials in the prescription ratio: 13～16 parts of Radix Aconiti Lateralis Preparatas (system), 5～8 parts of Radix Aconitis (system), 2～4 parts of Cortex Cinnamomis, 9～12 parts of Radix Codonopsis, 9～12 parts of Radix Angelicae Sinensis, 9～12 parts of the Radix Paeoniae Albas (stir-fry), 9～12 parts of Herba Epimedii, 5～8 parts of Olibanums (system), by pulverizing medicinal materials;
B. the medical material after pulverizing is added to the water, soaks 30min, add water, heating and refluxing extraction 3 times, extracting liquid filtering, centrifugal, merge supernatant;
C. precipitate with ethanol: supernatant precipitates with ethanol;
D. extract purification: through absorption with macroporous adsorbent resin, the washing decontamination, ethanol elution, concentration and recovery ethanol, obtain compound extract;
E. the Polyethylene Glycol composite interstitial substance is put to heat fused in water-bath, after fusing, compound extract is added in substrate, constantly agitating heating, keep mixed liquor at the melting state, by impouring pill dripping machine hopper after its mix homogeneously, start stirring, adjusting splashes into speed, dripping bore, drips distance, then the mixed liquor of compound extract and substrate is splashed in condensing agent coolingly, finally takes out cooling drop pill, remove surperficial liquid coolant, air-dry and get final product.
Method as above, wherein, in step b, each amount of water is 6～10 times of medical material weight, each extraction time is at 0.5h～1.5h, the centrifugal 20～30min of 3000～5000r/min.
Method as above, wherein, in step c, the concentration of described ethanol is 65～85vt%.
Method as above, wherein, in steps d, described macroporous adsorbent resin is a kind of in D101, XAD-7, LSD001, DA-201, XAD-7 and AB-8, the concentration of eluting ethanol used is 30～95vt%, collects eluent, by the eluent concentrating under reduced pressure.
Method as above, wherein, in step e, described Polyethylene Glycol composite interstitial substance is PEG4000: PEG6000=1: the Polyethylene Glycol mixture of 7～12 (volume ratios); Compound extract mixes by 1: 2～4 weight ratio with described substrate; The described speed that splashes into is 30～45/min, and the dripping bore is 3～4mm, and dripping distance is 5～9cm; Described condensing agent is dimethicone, and the temperature of condensing agent is 2～8 ℃.
A kind of preparation method for the treatment of the compound traditional Chinese medicinal dripping pills of hyperosteogeny, it is to complete according to the following steps:
A. Chinese crude drug ratio: 7.4 parts of 14.8 parts of Radix Aconiti Lateralis Preparatas (system), 7.4 parts of Radix Aconitis (system), 3.7 parts of Cortex Cinnamomis, 11.1 parts of Radix Codonopsis, 11.1 parts of Radix Angelicae Sinensis, 11.1 parts of the Radix Paeoniae Albas, 11.1 parts of Herba Epimedii, Olibanum take ingredients, pulverize 10～20 order powder;
B. the medical material after pulverizing is added to the water, soaks 30min, heating and refluxing extraction 3 times, amount of water is followed successively by 10,8,6 times of medical material weight, and extraction time is followed successively by 1.5h, 0.75h, 0.75h, extracting liquid filtering, 4000r/min, 20min is centrifugal, merges supernatant;
C. precipitate with ethanol: 75vt% ethanol precipitation for supernatant;
D. extract purification: a kind of absorption with macroporous adsorbent resin in D101, XAD-7, LSD001, DA-201, XAD-7 and AB-8, washing decontamination, 80vt% ethanol elution, eluent concentrating under reduced pressure;
E. by PEG4000: PEG6000=1: the Polyethylene Glycol composite interstitial substance of 9 (volume ratios) is put heat fused in water-bath;
F. compound extract and Polyethylene Glycol composite interstitial substance are mixed by the weight ratio of 1: 2.4, constantly agitating heating, control mixed liquor at the melting state, by its mix homogeneously;
G. keep the melting state, by mixed liquor impouring pill dripping machine hopper, start stirring;
H. regulate dripping bore 3mm, drip 40/min of speed, drip apart from 6cm;
I. the mixed liquor of compound extract and Polyethylene Glycol composite interstitial substance is splashed in condensing agent coolingly, described condensing agent is dimethicone, and the temperature of condensing agent is 2-8 ℃;
J. take out cooling drop pill, remove surperficial liquid coolant, air-dry and get final product.
The compound traditional Chinese medicinal dripping pills of the treatment hyperosteogeny prepared according to the method described above.
Beneficial effect of the present invention is:
1. the present invention has provided the dropping pill formulation of fugui ostealgia compound and the method for preparation thereof.Drop pill of the present invention has the effect of warming YANG to expel cold, benefiting QI for activating blood circulation, reducing swelling and alleviating pain, for yang deficiency cold-dampness type cervical vertebra and gonarthrosis.
2. project cost of supplementary product used is low, and the main effective ingredient peoniflorin dissolution in drop pill obviously increases.
3. drop pill has an advantage: can improve the bioavailability of insoluble drug, be conducive to the stripping of medicine, therefore bioavailability is higher.Drop pill is rapid-action, easily carry out quality control, thereby curative effect is better than conventional dosage forms, and price is higher.Next is that to prepare the equipment of drop pill simple, easy to operate; The operation of drop pill is few, with short production cycle, and production automation program is high, and labor intensity is low, and labor productivity is high, for new research space is opened up in the development of Chinese medicine.
4. with " pill, powder, extract and pellet " dosage form of system Chinese medicine, compare, it has the outstanding feature that other dosage forms do not possess, and meets people to basic demands such as modern medicines preparation " three is little " (consumption is little, side effect is little, toxicity little) " triple effect " (efficient, long-acting, quick-acting) " tripartites " (being convenient for carrying, facilitating medication, the convenient storage).
The accompanying drawing explanation
The standard curve that Fig. 1 is the effective ingredient peoniflorin.
Fig. 2 is for measuring the HPLC collection of illustrative plates of effective ingredient paeoniflorin content; The negative reference substance of Fig. 2 A, Fig. 2 B is compound dripping pill of the present invention.
The release in vitro curve that Fig. 3 is compound dripping pill of the present invention and tablet.
The specific embodiment
(1) compound recipe extracts:
The Chinese crude drug ratio: Radix Aconiti Lateralis Preparata (system) 14.8g, Radix Aconiti (system) 7.4g, Cortex Cinnamomi 3.7g, Radix Codonopsis 11.1g, Radix Angelicae Sinensis 11.1g, Radix Paeoniae Alba 11.1g, Herba Epimedii 11.1g, Olibanum 7.4g take ingredients, are ground into 20 order powder.Chinese medicine is placed in to extraction pot, adds the water of 9 times of medical material total amounts, heated and boiled 1.5h, filtered while hot.Repeat above-mentioned steps, in filtering residue, add 7 times of water, boil filtered while hot after 50min.Continue to repeat above-mentioned steps, in filtering residue, add 5 times of water, filter after boiling 30min.Merge three times filtrate, put in large capacity centrifuge, the centrifugal 30min of 4000r/min, abandon precipitation.
(2) precipitate with ethanol: supernatant precipitates with 80vt% ethanol.
(3) extract purification: precipitate, through macroporous adsorbent resin D101 absorption, is washed decontamination.The 65vt% ethanol elution, concentration and recovery ethanol, ethanol relative density 1.35 (50-60 ℃), obtain compound extract.
(4) preparation of compound dripping pill:
By PEG4000: PEG6000=1: 7 Polyethylene Glycol composite interstitial substance is put heat fused in water-bath, after fusing, by compound extract, the weight ratio by 1: 2 adds in substrate, continuous agitating heating, control 51 ± 5 ℃ of temperature, keep mixed liquor at the melting state, by after its mix homogeneously, keep in temperature impouring pill dripping machine hopper, start stirring, regulate and to splash into 45/min of speed, dripping bore 3mm, drip apart from 5cm, then splash in the dimethicone of 2 ℃ of condensing agents cooling.Finally take out cooling drop pill, remove surperficial liquid coolant, air-dry and get final product.
Embodiment 2
(1) compound recipe extracts:
The Chinese crude drug ratio: Radix Aconiti Lateralis Preparata (system) 14.8g, Radix Aconiti (system) 7.4g, Cortex Cinnamomi 3.7g, Radix Codonopsis 11.1g, Radix Angelicae Sinensis 11.1g, Radix Paeoniae Alba 11.1g, Herba Epimedii 11.1g, Olibanum 7.4g take ingredients, pulverize 20 order powder.Chinese medicine is placed in to extraction pot, adds the water of 6 times of medical material total amounts, heated and boiled 1.5h, filtered while hot.Repeat above-mentioned steps, will add filtered while hot after 7 times of water boil 50min in filtering residue.Continue to repeat above-mentioned steps, filter add 5 times of water boil 30min in filtering residue after.Merge three times filtrate, put in large capacity centrifuge, the centrifugal 30min of 3500r/min, abandon precipitation.
(2) precipitate with ethanol: supernatant precipitates with 75vt% ethanol.
(3) extract purification: through macroporous adsorbent resin XAD-7 absorption, the washing decontamination.The 80vt% ethanol elution, the eluent concentrating under reduced pressure.
(4) preparation of compound dripping pill:
By PEG4000: PEG6000=1: 8 Polyethylene Glycol composite interstitial substance is put heat fused in water-bath, after fusing, by compound extract, the weight ratio by 1: 3 adds in substrate, continuous agitating heating, control 53 ± 5 ℃ of temperature, keep mixed liquor at the melting state, by after its mix homogeneously, keep in temperature impouring pill dripping machine hopper, start stirring, regulate and to splash into 30/min of speed, dripping bore 3mm, drip apart from 6cm, then splash in the dimethicone of 5 ℃ of condensing agents cooling.Finally take out cooling drop pill, remove surperficial liquid coolant, air-dry and get final product.
Embodiment 3
(1) compound recipe extracts:
The Chinese crude drug ratio: Radix Aconiti Lateralis Preparata (system) 14.8g, Radix Aconiti (system) 7.4g, Cortex Cinnamomi 3.7g, Radix Codonopsis 11.1g, Radix Angelicae Sinensis 11.1g, Radix Paeoniae Alba 11.1g, Herba Epimedii 11.1g, Olibanum 7.4g take ingredients, pulverize 20 order powder.Chinese medicine is placed in to extraction pot, adds the water of 10 times of medical material total amounts, heated and boiled 1.5h, filtered while hot.Repeat above-mentioned steps, will add filtered while hot after 10 times of water boil 1h in filtering residue.Continue to repeat above-mentioned steps, filter add 6 times of water boil 30min in filtering residue after.Merge three times filtrate, put in large capacity centrifuge, the centrifugal 30min of 4600r/min, abandon precipitation.
(2) precipitate with ethanol: supernatant precipitates with 80vt% ethanol.
(3) extract purification: through macroporous adsorbent resin AB-8 absorption, the washing decontamination.The 65vt% ethanol elution, the eluent concentrating under reduced pressure.
(4) preparation of compound dripping pill:
By PEG4000: PEG6000=1: 11 Polyethylene Glycol composite interstitial substance is put heat fused in water-bath, after fusing, by compound extract, the weight ratio by 1: 2.5 adds in substrate, continuous agitating heating, control 49 ± 3 ℃ of temperature, keep mixed liquor at the melting state, by after its mix homogeneously, keep in temperature impouring pill dripping machine hopper, start stirring, regulate and to splash into 45/min of speed, dripping bore 4mm, drip apart from 9cm, then splash in the dimethicone of 8 ℃ of condensing agents cooling.Finally take out cooling drop pill, remove surperficial liquid coolant, air-dry and get final product.
Embodiment 4
(1) compound recipe extracts:
The Chinese crude drug ratio: Radix Aconiti Lateralis Preparata (system) 14.8g, Radix Aconiti (system) 7.4g, Cortex Cinnamomi 3.7g, Radix Codonopsis 11.1g, Radix Angelicae Sinensis 11.1g, Radix Paeoniae Alba 11.1g, Herba Epimedii 11.1g, Olibanum 7.4g take ingredients, pulverize 15 order powder.Chinese medicine is placed in to extraction pot, adds the water of 9 times of medical material total amounts, heated and boiled 1.5h, filtered while hot.Repeat above-mentioned steps, will add filtered while hot after 9 times of water boil 1h in filtering residue.Continue to repeat above-mentioned steps, filter add 6 times of water boil 30min in filtering residue after.Merge three times filtrate, put in large capacity centrifuge, the centrifugal 26min of 4800r/min, abandon precipitation.
(2) precipitate with ethanol: supernatant precipitates with 70vt% ethanol.
(3) extract purification: through macroporous adsorbent resin XAD-7 absorption, the washing decontamination.The 68vt% ethanol elution, the eluent concentrating under reduced pressure.
(4) preparation of compound dripping pill:
By PEG4000: PEG6000=1: 12 Polyethylene Glycol composite interstitial substance is put heat fused in water-bath, after fusing, by compound extract, the weight ratio by 1: 4 adds in substrate, continuous agitating heating, control 53 ± 3 ℃ of temperature, keep mixed liquor at the melting state, by after its mix homogeneously, keep in temperature impouring pill dripping machine hopper, start stirring, regulate and to splash into 40/min of speed, dripping bore 3mm, drip apart from 5cm, then splash in the dimethicone of 7 ℃ of condensing agents cooling.Finally take out cooling drop pill, remove surperficial liquid coolant, air-dry and get final product.
Embodiment 5
(1) compound recipe extracts:
The Chinese crude drug ratio: Radix Aconiti Lateralis Preparata (system) 14.8g, Radix Aconiti (system) 7.4g, Cortex Cinnamomi 3.7g, Radix Codonopsis 11.1g, Radix Angelicae Sinensis 11.1g, Radix Paeoniae Alba 11.1g, Herba Epimedii 11.1g, Olibanum 7.4g take ingredients, pulverize 20 order powder.Chinese medicine is placed in to extraction pot, adds the water of 10 times of medical material total amounts, heated and boiled 1.5h, filtered while hot.Repeat above-mentioned steps, will add filtered while hot after 10 times of water boil 1h in filtering residue.Continue to repeat above-mentioned steps, filter add 6 times of water boil 30min in filtering residue after.Merge three times filtrate, put in large capacity centrifuge, the centrifugal 25min of 3500r/min, abandon precipitation.
(2) precipitate with ethanol: supernatant precipitates with 78vt% ethanol.
(3) extract purification: through macroporous adsorbent resin DS-8 absorption, the washing decontamination.The 75vt% ethanol elution, the eluent concentrating under reduced pressure.
(4) preparation of compound dripping pill:
By PEG4000: PEG6000=1: 11 Polyethylene Glycol composite interstitial substance is put heat fused in water-bath, after fusing, by compound extract, the weight ratio by 1: 3.5 adds in substrate, continuous agitating heating, control 52 ± 5 ℃ of temperature, keep mixed liquor at the melting state, by after its mix homogeneously, keep in temperature impouring pill dripping machine hopper, start stirring, regulate and to splash into 35/min of speed, dripping bore 2mm, drip apart from 4cm, then splash in the dimethicone of 7 ℃ of condensing agents cooling.Finally take out cooling drop pill, remove surperficial liquid coolant, air-dry and get final product.
Embodiment 6
(1) compound recipe extracts:
The Chinese crude drug ratio: Radix Aconiti Lateralis Preparata (system) 14.8g, Radix Aconiti (system) 7.4g, Cortex Cinnamomi 3.7g, Radix Codonopsis 11.1g, Radix Angelicae Sinensis 11.1g, Radix Paeoniae Alba 11.1g, Herba Epimedii 11.1g, Olibanum 7.4g take ingredients, pulverize 10 order powder.Chinese medicine is placed in to extraction pot, adds the water of 10 times of medical material total amounts, heated and boiled 1.5h, filtered while hot.Repeat above-mentioned steps, will add filtered while hot after 7 times of water boil 1h in filtering residue.Continue to repeat above-mentioned steps, filter add 6 times of water boil 30min in filtering residue after.Merge three times filtrate, put in large capacity centrifuge, the centrifugal 25min of 3800r/min, abandon precipitation.
(2) precipitate with ethanol: supernatant precipitates with 81vt% ethanol.
(3) extract purification: through macroporous adsorbent resin DA-201 absorption, the washing decontamination.The 65vt% ethanol elution, the eluent concentrating under reduced pressure.
(4) preparation of compound dripping pill:
By PEG4000: PEG6000=1: 8 Polyethylene Glycol composite interstitial substance is put heat fused in water-bath, after fusing, by compound extract, the weight ratio by 1: 3 adds in substrate, continuous agitating heating, control 50 ± 3 ℃ of temperature, keep mixed liquor at the melting state, by after its mix homogeneously, keep in temperature impouring pill dripping machine hopper, start stirring, regulate and to splash into 40/min of speed, dripping bore 3mm, drip apart from 3.5cm, then splash in the dimethicone of 6 ℃ of condensing agents cooling.Finally take out cooling drop pill, remove surperficial liquid coolant, air-dry and get final product.
Embodiment 7
(1) compound recipe extracts:
The Chinese crude drug ratio: Radix Aconiti Lateralis Preparata (system) 14.8g, Radix Aconiti (system) 7.4g, Cortex Cinnamomi 3.7g, Radix Codonopsis 11.1g, Radix Angelicae Sinensis 11.1g, Radix Paeoniae Alba 11.1g, Herba Epimedii 11.1g, Olibanum 7.4g take ingredients, pulverize 10 order powder.Chinese medicine is placed in to extraction pot, adds the water of 8 times of medical material total amounts, heated and boiled 1.5h, filtered while hot.Repeat above-mentioned steps, will add filtered while hot after 7 times of water boil 1h in filtering residue.Continue to repeat above-mentioned steps, filter add 6 times of water boil 30min in filtering residue after.Merge three times filtrate, put in large capacity centrifuge, the centrifugal 30min of 3000r/min, abandon precipitation.
(2) precipitate with ethanol: supernatant precipitates with 75vt% ethanol.
(3) extract purification: through macroporous adsorbent resin LSD001 absorption, the washing decontamination.The 77vt% ethanol elution, the eluent concentrating under reduced pressure.
(4) preparation of compound dripping pill:
By PEG4000: PEG6000=1: 11 Polyethylene Glycol composite interstitial substance is put heat fused in water-bath, after fusing, by compound extract, the weight ratio by 1: 2.8 adds in substrate, continuous agitating heating, control 51 ± 3 ℃ of temperature, keep mixed liquor at the melting state, by after its mix homogeneously, keep in temperature impouring pill dripping machine hopper, start stirring, regulate and splash into 42/min of speed, dripping bore 4mm, drip apart from 2.5cm, then splash in 6 ℃ of dimethicones of condensing agent cooling.Finally take out cooling drop pill, remove surperficial liquid coolant, air-dry and get final product.
Embodiment 8
(1) compound recipe extracts:
The Chinese crude drug ratio: Radix Aconiti Lateralis Preparata (system) 14.8g, Radix Aconiti (system) 7.4g, Cortex Cinnamomi 3.7g, Radix Codonopsis 11.1g, Radix Angelicae Sinensis 11.1g, Radix Paeoniae Alba 11.1g, Herba Epimedii 11.1g, Olibanum 7.4g take ingredients, pulverize 20 order powder.Chinese medicine is placed in to extraction pot, adds the water of 9 times of medical material total amounts, heated and boiled 1.5h, filtered while hot.Repeat above-mentioned steps, will add filtered while hot after 8 times of water boil 1h in filtering residue.Continue to repeat above-mentioned steps, filter add 6 times of water boil 30min in filtering residue after.Merge three times filtrate, put in large capacity centrifuge, the centrifugal 30min of 3500r/min, abandon precipitation.
(2) precipitate with ethanol: supernatant precipitates with 85vt% ethanol.
(3) extract purification: through macroporous adsorbent resin LS-300 absorption, the washing decontamination.The 79vt% ethanol elution, the eluent concentrating under reduced pressure.
(4) preparation of compound dripping pill:
By PEG4000: PEG6000=1: 8 Polyethylene Glycol composite interstitial substance is put heat fused in water-bath, after fusing, by compound extract, the weight ratio by 1: 2.5 adds in substrate, continuous agitating heating, control 52 ± 3 ℃ of temperature, keep mixed liquor at the melting state, by after its mix homogeneously, keep in temperature impouring pill dripping machine hopper, start stirring, regulate and to splash into 46/min of speed, dripping bore 3mm, drip apart from 7cm, then splash in the dimethicone of 4 ℃ of condensing agents cooling.Finally take out cooling drop pill, remove surperficial liquid coolant, air-dry and get final product.
Embodiment 9
The quality standard of drop pill
(1) profile: drop pill is solid harder, circular.
(2) ball weight: when the dropper bore within the specific limits, the caliber greatly drop pill of dripping is also large, otherwise little.Substrate forms the surface tension temperature influence after solution, therefore temperature is also heavy relevant with ball.Temperature rises, and surface tension reduces, and ball heavily reduces, and temperature descends, and surface tension increases, and ball is heavy also to be increased.
From with extracting 100 a collection of fugui ostealgia compound drop pill, claiming its gross weight, repeated trials 6 times, draw meansigma methods, calculates the approximate weight of every drop pill at random, and experimental result is in Table 1:
The table 1 ball test result of resurveying
(3) roundness: the translational speed of drop in condensing agent is faster, is subject to the impact of gravity and buoyancy larger, more easily is flat.Show that through test drop and condensing agent density differ greatly or the viscosity hour of condensing agent can increase translational speed, finally affect its roundness.
At random from a collection of fugui ostealgia compound drop pill, extract 1000 detect the substandard products numbers (the substandard products standard as: hangover is arranged, be flat, cavity etc. is arranged), substandard products shared ratio value in sum wherein, repeated trials 6 times, average, draw the substandard products number in every 1000, experimental result is in Table 2:
Table 2 roundness test result
From table 2: produce in 1000 drop pill and contain 23.6 of defective works, qualification rate reaches 97.64%.
Test definite moulding process according to this, 6 batches of fugui ostealgia compound drop pill of continuous production, measure and investigate through many indexes such as, dissolve scattered time limit different to outward appearance roundness, the ball method of double differences and stability, all meet " the pertinent regulations under Chinese Pharmacopoeia 2005 version " drop pill " item, show thus, this moulding process is feasible.
Radix Paeoniae Alba total glycosides assay in compound dripping pill
Take octadecylsilane chemically bonded silica as filler; Acetonitrile-0.1wt% the phosphoric acid solution (weight ratio 14: 86) of take is mobile phase; The detection wavelength is 230nm; 40 ℃ of column temperatures; Flow velocity 1mLmin
-1.
(1) preparation of reference substance solution
Precision takes peoniflorin reference substance 2.4mg, puts in the 10mL volumetric flask, adds methanol to scale, shakes up, and obtains peoniflorin reference substance mother solution.
(2) linear relationship
Accurate reference substance mother solution 0.2,0.3,0.4,0.5,0.6,0.7, the 0.8mL of drawing, put in the 10mL volumetric flask, add the methanol top and hold to scale, shake up, respectively in injecting chromatograph, carry out the HPLC detection, take sample size as abscissa X, peak area is vertical coordinate Y, carry out linear regression, its range of linearity is 0.048～0.192mg, and regression equation is: Y=489155X-2540.9, r=0.9995.Result is as shown in the standard curve of table 3 and Fig. 1.
Table 3 reference substance mother solution linear dependence experimental result
(3) precision test
Get and pipette the solution that the reference substance mother solution is 0.3mL, repeat sample introduction 5 times, by calculated by peak area, obtain precision RSD=1.23%, illustrate that its precision is good.Experimental result is in Table 4.
Table 4 reference substance mother solution precision test
| |
1 | 2 | 3 | 4 | 5 | RSD％ |
| Peak area | 31861.97 | 31078.25 | 32096.14 | 31902.37 | 31753.69 | 1.23 |
(4) stability
The solution that to get the reference substance mother solution be 0.3mL places respectively 2,4,6,8,10h is measured, and peak area is followed successively by 31761.97,32235.15,31252.39,30581.64,30213.67, RSD=2.65%, result shows that need testing solution is good at the 10h internal stability.
(5) blank assay
The preparation of blank solution is in the ratio of prescription taste of Chinese medicine, autogamy, containing group's medicine of Radix Paeoniae Alba, is not made blank preparation by technique, by content assaying method, prepares blank solution, measure as stated above, blank solution does not show chromatographic peak with the peoniflorin reference substance at identical retention time place as a result.The HPLC collection of illustrative plates of blank product as shown in Figure 2 A.
(6) assay
Get the about 0.3g of drop pill of the present invention, accurately weighed, smash to pieces, put in the 25mL measuring bottle, add dissolve with methanol, supersound process (power 240W, frequency 45kHz) 60min, take out, place cooling, centrifugal (2500r/min, 20min), add methanol constant volume to scale, shake up, filter, get subsequent filtrate, obtain.The HPLC collection of illustrative plates of drop pill of the present invention is as shown in Fig. 2 B, and in figure, 1 place, peak is peoniflorin, and calculating paeoniflorin content by standard curve is 0.507mg/g.
Embodiment 11
Vitro release is measured
Getting three batches of drop pill, marketed tablet is placed in respectively and turns basket and carry out the vitro release investigation.The hydrochloric acid solution 900mL of 0.9vt% of take is release medium, and turning the basket rotating speed is 100rmin
-1, temperature (37 ± 0.5) ℃, through 2h, will turn basket emersion liquid level immediately, get liquid 5mL and detect the wherein content of peoniflorin; Discard acid solution, with being about to turn basket, to immerse the 900mL potassium dihydrogen phosphate-borate buffer solution (pH6.8) that is preheated to (37 ± 0.5) ℃ be dissolution medium, rotating speed 100rmin
-1, respectively at 15,30,45,60,75,90,105,120min sampling 5mL, through the 0.8m filter membrane, filter, after getting the suitable dilution of subsequent filtrate 0.2 μ L, 20 μ L sample introductions, calculate burst size percent.
Supplement the 5mL fresh medium after every sub-sampling.Result is as shown in table 5 and Fig. 3.
Visible, the burst size of three batches of compound recipe drop pill and commercially available compound tablet 2h in acid all is less than 10%, meets " the pertinent regulations of Chinese pharmacopoeia.And, in the PBS of pH6.8, discharge in drop pill 15min and surpass 45%, 60min and surpass 80%, basically all discharge, compare rate of release be significantly improved (P<0.05) with tablet.
Table 5 drop pill and marketed tablet discharge (n=3) in acid solution
Claims (3)
1. a preparation method for the treatment of the compound traditional Chinese medicinal dripping pills of hyperosteogeny, is characterized in that, completes according to the following steps:
A. take following medicinal materials by following part by weight: 13～16 parts of Radix Aconiti Lateralis Preparatas, 5～8 parts of Radix Aconitis, 2～4 parts of Cortex Cinnamomis, 9～12 parts of Radix Codonopsis, 9～12 parts of Radix Angelicae Sinensis, 9～12 parts of the Radix Paeoniae Albas, 9～12 parts of Herba Epimedii, 5～8 parts of Olibanums, by pulverizing medicinal materials;
B. the medical material after pulverizing is added to the water and soaks 30min, add water, heating and refluxing extraction 3 times, extracting liquid filtering, centrifugal, merge supernatant;
C. precipitate with ethanol: supernatant is precipitated with ethanol;
D. extract purification: precipitate is through absorption with macroporous adsorbent resin, the washing decontamination, and ethanol elution, concentration and recovery ethanol, obtain compound extract;
E. the Polyethylene Glycol composite interstitial substance is put to heat fused in water-bath, after fusing, compound extract is added in substrate, constantly agitating heating, keep mixed liquor at the melting state, by impouring pill dripping machine hopper after its mix homogeneously, start stirring, adjusting splashes into speed, dripping bore, drips distance, then the mixed liquor of compound extract and substrate is splashed in condensing agent coolingly, finally takes out cooling drop pill, remove surperficial liquid coolant, air-dry and get final product;
Wherein, in step c, the concentration of described ethanol is 65～85vt%;
In steps d, described macroporous adsorbent resin is a kind of in D101, XAD-7, LSD001, DA-201, DS-8, LS-300 and AB-8, and the concentration of eluting ethanol used is 30～95vt%;
In step e, the Polyethylene Glycol mixture that the volume ratio that described Polyethylene Glycol composite interstitial substance is PEG4000 and PEG6000 is 1:7～12; Compound extract mixes by the weight ratio of 1:1～4 with described substrate; The described speed that splashes into is 30～45/min, and the dripping bore is 3～4mm, and dripping distance is 5～9cm; Described condensing agent is dimethicone, and the temperature of condensing agent is 2～8 ℃.
2. method according to claim 1, is characterized in that, in step b, each amount of water is 6～10 times of medical material weight, and each extraction time, centrifugal rotational speed was 3000～5000r/min at 0.5h～1.5h, and centrifugation time is 20～30min.
3. the compound traditional Chinese medicinal dripping pills of the treatment hyperosteogeny prepared according to the described method of claim 1.
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| CN1418668A (en) * | 2002-11-26 | 2003-05-21 | 贵州家诚药业有限责任公司 | Chinese patent drug for treating bone ache, and its prepn. method |
| CN1528415A (en) * | 2003-10-17 | 2004-09-15 | 陕西康惠制药有限公司 | Capsule for treating cervical spondylosis and hyperplastic arthritis and preparing process thereof |
| CN101579390A (en) * | 2008-05-15 | 2009-11-18 | 北京北大维信生物科技有限公司 | Medicinal dripping pill for treating osteoporosis |
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| CN1418668A (en) * | 2002-11-26 | 2003-05-21 | 贵州家诚药业有限责任公司 | Chinese patent drug for treating bone ache, and its prepn. method |
| CN1528415A (en) * | 2003-10-17 | 2004-09-15 | 陕西康惠制药有限公司 | Capsule for treating cervical spondylosis and hyperplastic arthritis and preparing process thereof |
| CN101579390A (en) * | 2008-05-15 | 2009-11-18 | 北京北大维信生物科技有限公司 | Medicinal dripping pill for treating osteoporosis |
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| Title |
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| 郑来丽.附桂骨痛复方提取工艺及其初步药效学研究.《中国优秀硕士学位论文全文数据库 医药卫生科技辑》.2010,(第7期),29-40页. |
| 附桂骨痛复方提取工艺及其初步药效学研究;郑来丽;《中国优秀硕士学位论文全文数据库 医药卫生科技辑》;20100715(第7期);29-40页 * |
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