CN104069170A - Preparation method of Huodan dropping pills - Google Patents
Preparation method of Huodan dropping pills Download PDFInfo
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- CN104069170A CN104069170A CN201410301910.3A CN201410301910A CN104069170A CN 104069170 A CN104069170 A CN 104069170A CN 201410301910 A CN201410301910 A CN 201410301910A CN 104069170 A CN104069170 A CN 104069170A
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Abstract
The invention relates to a preparation method of Huodan dropping pills. The method comprises the following steps: respectively putting a raw material hyocholic acid sieved by a 60-mesh sieve and an auxiliary material polyethylene glycol 6000 according to a prescription quantity into a mixer for fully mixing, throwing the mixed material into a melting tank and melting in a heating manner so as to obtain an evenly-dispersed undertint medicine liquid while the medium is molten; adding patchouli oil in a specified prescription quantity in a stirring state; evenly stirring the medicine liquid for forming dropping pills; then, dropping the medicine liquid into cooling oil array pipes with certain temperature gradients in a speed control manner under a certain heat preservation condition; and collecting the formed dropping pills, centrifugally removing the cooling oil and collecting the dropping pills. According to the method, the dropping temperature cannot exceed 85 DEG C, so that the volatilization loss of the patchouli oil taken as an effective medicine is obviously reduced. Compared with a powdery feeding process, according to the method provided by the invention, the heating time of the materials is shorted by half.
Description
Technical field
The present invention relates to solid dispersion pharmaceutical preparation, be specifically related to the technical field that a kind of leaves of pulse plants gallbladder method for preparing drop pills belongs to Chinese medicine preparation.
Background technology
Drop pill is a kind of solid dispersion (Soild dispertion).So-called solid dispersion refers to that material dispersed (comprising various states of matters) is dispersed in a kind of compounding substances that solid state medium forms, material dispersed can dispersion with state molecule, ion or microgranule wherein.Solid dispersion is widely used in modern pharmaceutical as a kind of drug-supplying system, after solid or liquid medicine and substrate heat fused mix, splashes in not miscible condensed fluid, shrinks condensation and the preparation made, mainly supplies oral application.This dripping method pelletizing process, is actually the form of solid dispersion being made to drop pill.
Dropping preparation method pill starts from vitamin A, D ball prepared by Denmark pharmaceutical factory in 1933.Domesticly start from 1958.In recent years, the application of synthetic, semi-synthetic substrate and solid dispersion technology makes drop pill have development rapidly, particularly in the exploitation of new product of Chinese medicine, has obtained very large development." Chinese Pharmacopoeia " version in 1977 takes the lead in recording drops, nineteen ninety-five, version recorded 9 kinds of drop pills, version in 2000, version in 2005 and version in 2010 are obvious increases, the Chinese medicine dripping pills authentication code that existing State Food and Drug Administration issues has nearly 100 kinds, wherein has more than 20 to plant for the Chinese medicine dripping pills of cardiovascular system.
Traditional Chinese Medicine Dropping Pill is subject to people's attention just day by day, it has adopted Western medicine advanced person's preparation hands section, the drop pill of preparing with solid dispersion technology is that a kind of Chinese medicine preparation fully contacts with mucomembranous surface, Effective Component of Chinese Medicine is by mucosa upper surface Cell uptake, directly enter the Chinese patent medicine preparation dosage form of the administering mode of people's blood circulation, its outstanding feature is as directly absorbed and enter blood circulation without liver, effectively avoid first pass effect, there is curative effect rapid, bioavailability is high, side effect is little, medication is feature sublingual administration easily, absorb better, onset is faster.
Leaves of pulse plants gallbladder drop pill at first by Shanghai Chinese medicine one factory the end of the seventies, researched and developed the novel form forming on ancient prescription " liver heat removing protect brain ball " (another name HUODAN WAN) basis, its punishment is made up of hyocholic acid and patchouli oil (Pogostemon cablin) two taste medicines, there is heat clearing awayization turbid, a surname's clearing the nasal passage effect, for wind and cold heat-transformation, on gallbladder fire, attack the nasal obstruction causing and owe logical, nasosinusitis headache.
Existing leaves of pulse plants gallbladder drop pill quality standard records in the department of otorhinolaryngology department of dermatologry fascicle in Chinese patent medicine provincial standard rising national standard part, standard that what it was up-to-date become a full member has been done correction to prescription flavour of a drug title, and " oil of Herba Pogostemonis " before amendment is " patchouli oil " (WS-11486 (ZD-1486)-2002-2012Z).In standard, having binomial to differentiate, is respectively that thin layer is differentiated patchouli alcohol in oil of Herba Pogostemonis and the Hyodeoxycholic Acid in hyocholic acid; To adopt thin layer chromatography scanning to detect the Hyodeoxycholic Acid (>=2.7mg/ ball) in hyocholic acid containing surveying.
The preparation method of leaves of pulse plants gallbladder drop pill is first with a small amount of ethanol heating for dissolving hyocholic acid, then join in the polyethylene glycol 6000 having melted and fully and mix, finally add patchouli oil, after mixing, splash into molding in cooling dimethicone medium, remove surperficial oil stain, to obtain final product.
In above-mentioned standard technology, use a small amount of ethanol, but ethanol is herein not as drug prescription composition, and is only for hyocholic acid is first played to hydrotropy effect.The Hyodeoxycholic Acid of practical situation after by hydrotropy joins the Polyethylene Glycol of fusing and be uniformly mixed 0.5-1 hour under keeping warm mode, and in feed liquid, most of ethanol can be volatilized, but can confirm that ethanol still can be detained in drop pill.The existence of ethanol can make the cohesiveness of drop pill medium decline, cause dropping pill formulation hardness partially soft frangible, more disadvantageously make drop pill dissolve scattered time limit extend, this makes leaves of pulse plants gallbladder drop pill under legal process conditions be difficult to reach the technical requirement of dropping pill formulation new standard (dropping pill formulation standard had improved in country in 2005, specified when its dissolve scattered time limit is measured to add baffle plate).
Experiment showed, that the method that reduces amount of alcohol added or do not add ethanol prepares leaves of pulse plants gallbladder drop pill, can solve the quality problems such as partially soft, dissolve scattered time limit prolongation of drop pill, but this still has inconvenience and unfavorable factor in actual production operation.
Taking " adding less ethanol " as example, first with ethanol, hyocholic acid is in harmonious proportion to pulping, then in a continuous manner, slowly put in the Polyethylene Glycol having melted, for making the dispersed normal needization long period of hyocholic acid.
If " not adding ethanol " scheme of employing; feed intake with hyocholic acid powder body; because can making this raw material, the water-insoluble feature of hyocholic acid floats on Polyethylene Glycol liquid level; thereby force the powder body process that feeds intake to add with slower speed; dissolve dispersion effect in order to improve hyocholic acid simultaneously; often can suitably improve Polyethylene Glycol holding temperature; this brings potential danger also can to the safety of medicine itself; because Polyethylene Glycol can produce thermal-oxidative degradation more than 100 DEG C; produce formic acid compound and carboxylate, in first acidization wherein, can generate with formaldehyde intermediate.
Obviously how under non high temperature state, to shorten hyocholic acid solution time and adjuvant Polyethylene Glycol heated time is the problem that the present invention will pay close attention to.
Summary of the invention
The object of the invention is to, a kind of leaves of pulse plants gallbladder method for preparing drop pills is provided, to overcome the existing above-mentioned shortcoming and defect of prior art.
The present invention's operating sequence of breaking the normal procedure, has proposed low-temperature mixed-thawing integral process.So-called low temperature " mix-melt " is integrated refers to that the polyethylene glycol 6000 of hyocholic acid raw material and powdery is fully mixed in advance, then feeds intake, low-temperature heat thawing, gets final product to obtain homodisperse hyocholic acid Polyethylene Glycol liquid.Add subsequently patchouli oil just can start the preparation of drop pill, the temperature of whole technical process is controlled at 70-85 DEG C, avoids higher than 100 DEG C.
The technical problem that will solve required for the present invention, can be achieved through the following technical solutions:
A kind of leaves of pulse plants gallbladder method for preparing drop pills, is characterized in that, comprises the following steps:
(1) get respectively hyocholic acid raw material and Polyethylene Glycol adjuvant, put into mixer, fully mix, make mixed material;
(2) mixed material of being prepared by step (1) drops in melting cylinder, and heat fused obtains finely dispersed light medicinal liquid at fusing medium simultaneously;
(3) under stirring, add patchouli oil, make drop pill medicinal liquid, by even drop pill medicinal liquid agitating;
(4) by drop pill medicinal liquid under heat-retaining condition, control and drip speed, splash in the cold oil tubulation of thermograde, collect molding drop pill;
(5) centrifugal removal cold oil, collects drop pill, i.e. finished product.
In step (1), described hyocholic acid is 60 object powder, and consumption is 2~3kg.Described Polyethylene Glycol is the polyethylene glycol 6000 g/mol of molecular mass, and consumption is 15~16kg.
In step (2), the temperature of described fusing is 70~85 DEG C.
In step (3), the amount 2~3kg of described patchouli oil.
In step (4), under 70~85 DEG C of heat-retaining conditions, start dripping.Described speed is 30~60 per minute.Described cold oil tubulation has thermograde, 30~40 DEG C of cooling oil surface temperatures, 3~5 DEG C of bottom temps.
Further, described cold oil tubulation is equipped with cold oil, and described cold oil adopts dimethicone, and kinematic viscosity is 100~150 centistoke (mm
2/ s).
Beneficial effect of the present invention:
The maximum feature of technique of the present invention is that Polyethylene Glycol fusing and hyocholic acid mixing are synchronously carried out, this had both shortened material heated time, can obtain at a lower temperature again finely dispersed stable emulsion medicinal liquid, thereby avoid the potentiality that high temperature has Polyethylene Glycol to destroy, guaranteed the safety of medicine itself.Because dripping temperature is no more than 85 DEG C, effectively the volatilization of flavour of a drug patchouli oil is wandered away and also can significantly be reduced.Compare with powder body charging technology, the present invention can make material heated time reduce by half.
Dissolve or disperse bad " worry " for hyocholic acid under cryogenic conditions, having done binomial process certification test.Get the drop pill medicinal liquid of preparing by new process, first under low temperature heat-retaining condition, leave standstill 3 hours, found that precipitation or lamination do not appear in drop pill medicinal liquid.This drop pill medicinal liquid is crossed 60 mesh sieves subsequently, and result medicinal liquid can pass through mesh screen, the emulsifying of drop pill medicinal liquid is described in order, and hyocholic acid is dispersed not to be a problem.
Detailed description of the invention
Below in conjunction with specific embodiment example, the present invention is done to progressive explanation.Should be understood that following examples example is only for the present invention is described but not for limiting scope of the present invention.
The leaves of pulse plants gallbladder drop pill quality evaluation of preparation technology's gained of the present invention is taking rules of preparations in current edition Chinese Pharmacopoeia (2010) as foundation, in conjunction with effective ingredient in this medicine: Hyodeoxycholic Acid, patchouli oil and patchouli alcohol assay are made comprehensive objective judgement.
In embodiment 1 leaves of pulse plants gallbladder drop pill, Hyodeoxycholic Acid is measured
Measure according to high performance liquid chromatography (2010 editions one annex VI D of Chinese Pharmacopoeia).
Chromatographic condition and system suitability test octadecylsilane chemically bonded silica are filler; Acetonitrile-0.1% glacial acetic acid (50:50) is mobile phase; Evaporative light scattering detector.Number of theoretical plate calculates and should be not less than 3500 with Hyodeoxycholic Acid peak.
The preparation precision of reference substance solution takes through the phosphorus pentoxide drying under reduced pressure Hyodeoxycholic Acid reference substance of 24 hours appropriate, accurately weighed, adds methanol and makes the solution of every 1ml containing 0.4mg, to obtain final product.
It is appropriate that this product under weight differential item is got in the preparation of need testing solution, and porphyrize, gets 0.1g, accurately weighed, puts in 25ml measuring bottle, add methanol 20ml, supersound process (power 300W, frequency 50kHz) 10 minutes, takes out, and lets cool, add methanol to scale, shake up, considered, get subsequent filtrate, to obtain final product.
Accurate reference substance solution 10 μ l and the 20 μ l of drawing of algoscopy, need testing solution 20 μ l, injection liquid chromatography, measures, and calculates with external standard two-point method logarithmic equation, to obtain final product.
In embodiment 2 leaves of pulse plants gallbladder drop pill, patchouli oil is measured
Measure according to gas chromatography (Chinese Pharmacopoeia annex VI E).
Capillary column taking 5% phenyl methyl polysiloxanes as immobile phase of chromatographic condition and system suitability (column length is as 30m, and internal diameter is 0.32mm, film thickness be 0.25 μ m); Column temperature is temperature programming: 120 DEG C of initial temperatures, keep 5 minutes, and be warming up to 170 DEG C with the speed of 10 DEG C per minute, keep 4 minutes; Detector temperature is 280 DEG C, and injector temperature is 280 DEG C; Split sampling, split ratio is 10:1.Number of theoretical plate calculates and should be not less than 5000 by patchouli oil peak.
The preparation of reference substance solution compares product with patchouli oil raw material, gets in right amount, accurately weighed, adds ethyl acetate and makes the solution of every 1ml containing 2mg, to obtain final product.
10 of this product are got in the preparation of need testing solution, accurately weighed, put in 25ml measuring bottle, with ethyl acetate ultrasonic dissolution and be diluted to scale, shake up, as need testing solution.
Algoscopy is accurate reference substance solution and the each 1 μ l of need testing solution of drawing respectively, inject gas chromatograph, and normalization method is measured, and to obtain final product.
Patchouli alcohol assay in embodiment 3 leaves of pulse plants gallbladder drop pill
Measure according to gas chromatography (annex VI E).
Capillary column taking 5% phenyl methyl polysiloxanes as immobile phase of chromatographic condition and system suitability (column length is as 30m, and internal diameter is 0.32mm, film thickness be 0.25 μ m); Column temperature is temperature programming: 120 DEG C of initial temperatures, keep 5 minutes, and be warming up to 170 DEG C with the speed of 10 DEG C per minute, keep 4 minutes; Detector temperature is 280 DEG C, and injector temperature is 280 DEG C; Split sampling, split ratio is 10:1.Number of theoretical plate calculates and should be not less than 5000 by patchouli alcohol peak.
It is appropriate that patchouli alcohol reference substance is got in the preparation of reference substance solution, accurately weighed, adds ethyl acetate and make the solution of every 1ml containing 0.6mg, to obtain final product.
10 of this product are got in the preparation of need testing solution, accurately weighed, put in 25ml measuring bottle, with ethyl acetate ultrasonic dissolution and be diluted to scale, shake up, as need testing solution.
Algoscopy is accurate reference substance solution and the each 1 μ l of need testing solution of drawing respectively, and inject gas chromatograph, measures, and to obtain final product.
Mix at 470 DEG C of embodiment-fusing integration system is for leaves of pulse plants gallbladder drop pill
Got respectively 60 object hyocholic acid raw materials and polyethylene glycol 6000 adjuvant 2kg and 16kg, and put into mixer, and fully mixed, mixed material drops in melting cylinder, and heat fused obtains finely dispersed light medicinal liquid at fusing medium simultaneously.Under stirring, add 2kg patchouli oil, after stirring, under 70 DEG C of heat-retaining conditions, start dripping.Splash into and cooling, kinematic viscosity is housed as 100 centistoke (mm taking 50 speed per minute
2in/dimethicone colonnade s), 35 DEG C of cooling oil surface temperatures, 3 DEG C of bottom temps.Collect drop pill, remove top layer cold oil, can obtain finished product drop pill 19kg, yield 95%, ball focuses between 45-55mg, the heavy 50mg of average ball, dissolve scattered time limit 12 minutes, every of content is respectively 3.1mg, 4.2mg and 0.98 containing Hyodeoxycholic Acid, patchouli oil and patchouli alcohol.
Mix at 585 DEG C of embodiment-fusing integration system is for leaves of pulse plants gallbladder drop pill
All the other are with embodiment 1.
Mix at 6100 DEG C of embodiment-fusing integration system is for leaves of pulse plants gallbladder drop pill
All the other are with embodiment 1.
Embodiment 7 contrast tests: at 115 DEG C, tradition is prepared leaves of pulse plants gallbladder drop pill
All the other are with embodiment 1.
The test that embodiment 8 contrasts: at 130 DEG C, tradition is prepared leaves of pulse plants gallbladder drop pill
All the other are with embodiment 1.
New technology and old technique contrast test are all taked consistent ethanol (or adding less ethanol) scheme that do not add, and result of the test finds that drop pill has significant difference on outward appearance and total patchouli oil binomial, specifically sees the following form 1.
Table 1. the old and new technique sample quality comparative test result
Partially white in new technology sample appearance, and old powder body charging technology color sample is partially yellow; On total patchouli oil content, in new technology drop pill, guarantor's oil mass of patchouli oil is apparently higher than old technique sample.
By (40 DEG C of above-mentioned contrast test sample embodiment accelerated tests, 75% relative humidity), after January, observe and find, new technology (70, 85, 100 DEG C) three sample appearance color and lusters change without significance, still be yellowish translucent, but the sample appearance color and luster of preparing under 70 DEG C of conditions in old technique changes without significance, all the other 4 were yellow sample (85 originally, 100, 115 and 130 DEG C of techniques) but there is significant change, color and luster starts to turn to white, wherein 130 DEG C of technique sample whiting degree are the darkest, also find that drop pill sample has " chip " coming off simultaneously.There is whiting in the drop pill sample in accelerated test, has illustrated that in drop pill, volatile oil is wandered away.Volatile oil is that one group of homologue forms, and its volatilization rule is that the light oil heavy oil that gets ahead is careful.And patchouli alcohol (white solid) is " heavy oil " in patchouli oil volatile oil, volatilization is slow comparatively speaking, and " light oil " getting ahead can cause " heavy oil " patchouli alcohol content and be tending towards rising, and the measurement result of this and accelerated test sample matches.In view of the stability of Hyodeoxycholic Acid physicochemical property, this test does not contain survey to it.Concrete data are in table 2.
Table 2. the old and new technique sample accelerated test in January result
Sample index | Outward appearance | Total patchouli oil | Patchouli alcohol |
70 DEG C of new technologies | Yellow-white | 3.8mg/ grain | 1.15mg/ grain |
85 DEG C of new technologies | Yellow-white | 3.6 | 1.18 |
100 DEG C of new technologies | Light yellow | 3.4 | 1.21 |
70 DEG C of old techniques | Light yellow | 3.5 | 1.20 |
85 DEG C of old techniques | Light yellow | 2.8 | 1.22 |
100 DEG C of old techniques | Shallow white | 2.5 | 1.25 |
115 DEG C of old techniques | White | 2.4 | 1.40 |
130 DEG C of old techniques | White | 2.3 | 1.53 |
Analyze the reason that above-mentioned new, old technique sample quality changes, thinking the most basic is in drop pill preparation process due to heating temperature height and the variation of heated time length.
Above the specific embodiment of the present invention is illustrated, but the present invention is as limit, only otherwise depart from aim of the present invention, the present invention can also have various variations.
Claims (9)
1. a leaves of pulse plants gallbladder method for preparing drop pills, is characterized in that, comprises the following steps:
(1) get respectively hyocholic acid raw material and Polyethylene Glycol adjuvant, put into mixer, fully mix, make mixed material;
(2) mixed material of being prepared by step (1) drops in melting cylinder, and heat fused obtains finely dispersed light medicinal liquid at fusing medium simultaneously;
(3) under stirring, add patchouli oil, make drop pill medicinal liquid, by even drop pill medicinal liquid agitating;
(4) by drop pill medicinal liquid under heat-retaining condition, control and drip speed, splash in the cold oil tubulation of thermograde, collect molding drop pill;
(5) centrifugal removal cold oil, collects drop pill, i.e. finished product.
2. a kind of leaves of pulse plants gallbladder method for preparing drop pills according to claim 1, is characterized in that: in step (1), described hyocholic acid is 60 object powder, and consumption is 2~3kg.
3. a kind of leaves of pulse plants gallbladder method for preparing drop pills according to claim 1, is characterized in that: in step (1), and the polyethylene glycol 6000 g/mol that described Polyethylene Glycol is molecular mass, consumption is 15~16kg.
4. a kind of leaves of pulse plants gallbladder method for preparing drop pills according to claim 1, is characterized in that: in step (2), the temperature of described fusing is 70~85 DEG C.
5. a kind of leaves of pulse plants gallbladder method for preparing drop pills according to claim 1, is characterized in that: in step (3), and the amount 2~3kg of described patchouli oil.
6. a kind of leaves of pulse plants gallbladder method for preparing drop pills according to claim 1, is characterized in that: in step (4), under 70~85 DEG C of DEG C of heat-retaining conditions, start dripping.
7. a kind of leaves of pulse plants gallbladder method for preparing drop pills according to claim 1, is characterized in that: in step (4), described speed is 30~60 per minute.
8. a kind of leaves of pulse plants gallbladder method for preparing drop pills according to claim 1, is characterized in that: in step (4), described cold oil tubulation has thermograde 30~40 DEG C of cooling oil surface temperatures, 3~5 DEG C of bottom temps.
9. a kind of leaves of pulse plants gallbladder method for preparing drop pills according to claim 8, is characterized in that: described cold oil tubulation is equipped with cold oil, and described cold oil adopts dimethicone, and kinematic viscosity is 100~150 centistoke (mm
2/ s).
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Cited By (2)
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CN106539690A (en) * | 2015-09-18 | 2017-03-29 | 天士力制药集团股份有限公司 | A kind of continuous intelligent preparation method of liquid cooling drop pill |
CN113218480A (en) * | 2020-04-14 | 2021-08-06 | 浙江大学 | Characterization method of pill weight of dropping pills |
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CN1626134A (en) * | 2003-12-11 | 2005-06-15 | 天津天士力制药股份有限公司 | Medication for treating chronic rhinitis and nasal sinuitis |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106539690A (en) * | 2015-09-18 | 2017-03-29 | 天士力制药集团股份有限公司 | A kind of continuous intelligent preparation method of liquid cooling drop pill |
CN106539690B (en) * | 2015-09-18 | 2020-08-04 | 天士力医药集团股份有限公司 | Continuous intelligent preparation method of liquid cooling dropping pills |
CN113218480A (en) * | 2020-04-14 | 2021-08-06 | 浙江大学 | Characterization method of pill weight of dropping pills |
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