CN104398940B - Compound Momordica grosvenori cough-relieving piece preparation method - Google Patents
Compound Momordica grosvenori cough-relieving piece preparation method Download PDFInfo
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Abstract
The present invention disclose a kind of compound Momordica grosvenori cough-relieving piece preparation method, the Determination of Total Alkaloid of having added intermediate product of this method mainly in the preparation process of existing compound Momordica grosvenori cough stopping tablet, n-butanol extract assay.According to compound Momordica grosvenori cough stopping tablet steady quality produced by the present invention, it can make it that total alkaloid content reaches more than 1.0mg in every compound Momordica grosvenori cough stopping tablet of product, n-butanol extract content reaches up to more than 5.0%《Chinese Pharmacopoeia》Legal index in version one in 2010, it is possible to the effect of ensuring product compound Momordica grosvenori cough stopping tablet.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, especially a kind of compound Momordica grosvenori cough-relieving piece preparation method.
Background technology
Compound Momordica grosvenori cough stopping tablet is to use the related medicinal material recorded in NF to be prepared as raw material.It is existing
Compound Momordica grosvenori cough-relieving piece preparation method be by the way that each raw material are extracted respectively, obtain extracting cream, then mixing is equal
It is even, dry, it is tabletted to be eventually adding auxiliary material.But the preparation method there is it is very big the defects of --- finished product compound Momordica grosvenori
Cough-relieving tablet quality is unstable.Wherein,《Chinese Pharmacopoeia》Provided in versions one in 2010 every compound Momordica grosvenori cough stopping tablet effectively into
Total alkaloid in point must not be less than 1.0mg, the n-butanol extract content in every compound Momordica grosvenori cough stopping tablet active ingredient
5.0% must not be less than, although and its in the preparation method to prepare raw material species clear and definite, due to being not in every batch of raw material
What the alkaloid contained was just as, or due to its alkaloid extraction degree difference in leaching process, can all make
Active ingredient total alkaloid content in finished product compound Momordica grosvenori cough stopping tablet made from different batches, n-butanol extract content
Not necessarily arriving to reach《Chinese Pharmacopoeia》Legal index in version one in 2010, so as to result in finished product compound Momordica grosvenori cough-relieving
Tablet quality is unstable, and the effect of had a strong impact on compound Momordica grosvenori cough stopping tablet.
The content of the invention
The present invention provides a kind of compound Momordica grosvenori cough-relieving piece preparation method, in the method obtained compound Momordica grosvenori cough-relieving
Tablet quality is stable, and so that total alkaloid, n-butanol carry in the compound Momordica grosvenori cough stopping tablet active ingredient that final production obtains
The content of thing is taken to be attained by《Chinese Pharmacopoeia》Legal index in version one in 2010.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
This compound Momordica grosvenori cough stopping tablet is prepared by the raw material of following parts by weight:22.5 parts of Momordica grosvenori, the root bark of white mulberry 6
Part, 15 parts of the tuber of stemona, 88 parts of loguat leaf, 9 parts of Cynanchum glaucescens, 5.5 parts of balloonflower root;
Its preparation method comprises the following steps:
A. above-mentioned parts by weight are pressed, Momordica grosvenori is added water to cook 4 times, decoction liquor is then combined with and filters, be finally concentrated into
Relative density is 1.20, obtains Momordica grosvenori clear cream;
B. above-mentioned weight fraction is pressed, the root bark of white mulberry, the tuber of stemona, loguat leaf, Cynanchum glaucescens, balloonflower root are added water to cook 2 times, will be decocted twice
Boil liquid merges, filtered, concentration, and the ethanol for then adding 4 times of amounts of concentrate stir, and stand 48 hours, filter, concentrate
To the clear cream that relative density is 1.20;
C. the Momordica grosvenori clear cream that step A is obtained and the clear cream that step B is obtained are well mixed, dry, pulverize into powder, then
The powder is made to the particle of the mesh of 20 mesh~24;
D. added in the particle that step C is obtained and account for the magnesium stearate of the granular mass 0.5% and account for the granular mass
0.5% talcum powder, it is well mixed, then carries out the detection of Determination of Total Alkaloid and n-butanol extract, be finally pressed into
Piece, film coating obtain this compound Momordica grosvenori cough stopping tablet;Wherein, if found by measure per the total of powder described in 0.51g steps C
Alkaloid is less than 5.0% less than the 1.0mg n-butanol extract contents for either finding the particle by measure, then exists
The size of the compound Momordica grosvenori cough stopping tablet is adjusted during film-making so that the total alkaloid content of every compound Momordica grosvenori cough stopping tablet is not
It is not less than 5.0% less than 1.0mg, n-butanol extract content;If find total life per powder described in 0.51g steps C by measure
Alkaloids content finds that the n-butanol extract content of the particle is not less than 5.0% not less than 1.0mg and by measure, then is not required to
The size of the compound Momordica grosvenori cough stopping tablet is adjusted in film-making, the weight according to every compound Momordica grosvenori cough stopping tablet is 0.51
Gram carry out film-making;
In the above-mentioned technical solutions, more specifically technical scheme is:
Determination of Total Alkaloid method described in step C is:The powder in accurately weighed 10 grams of step C, adds 70% second
Alcohol 100ml is heated to reflux 2 times, 1 hour every time, filtration, merging filtrate, is evaporated to obtain residue, is added hydrochloric acid solution to make the residue
Dissolving, is transferred in 200ml volumetric flasks, adds hydrochloric acid solution to be settled to scale, shake up, and filters, discards primary filtrate, then adds again
Hydrochloric acid solution dissolves, and is transferred in another 200mL volumetric flask, adds hydrochloric acid solution to be settled to scale;Precision measures subsequent filtrate
50ml, put in separatory funnel, adjust pH value to 9~10 with ammonia solution, shake up, shake extraction 5 times with chloroform, every time
20ml, merge chloroform liquid, be washed with water 2 times, each 10ml, discard water lotion, chloroform liquid, which is put, to be dried to constant weight
In evaporating dish, it is evaporated, it is accurately weighed in 100 DEG C of dryings to constant weight, calculate, produce total alkaloid content;
The content assaying method of n-butanol extract is described in step D:Particle 3g described in step D is taken, it is finely ground, it is accurately weighed
2 grams, put in 250ml boiling flasks, precision adds n-butanol 50ml, weighed weight, is heated to reflux 1 hour, lets cool, then weighed heavy
Amount, the weight of less loss is supplied with n-butanol, is shaken up, is filtered with dry filter paper;Primary filtrate is discarded, precision draws subsequent filtrate 25ml,
Put and dry into the evaporating dish of constant weight, be evaporated, dried 3 hours at 105 DEG C, in dislocation drier, cooled down 30 minutes, rapid essence
Close weighed weight, calculate, produce the content of n-butanol extract.
Due to using above-mentioned technical proposal, the beneficial effect that the present invention obtains is:
According to compound Momordica grosvenori cough stopping tablet steady quality produced by the present invention, every compound Momordica grosvenori of product can be caused to stop
Total alkaloid content reaches more than 1.0mg in cough piece, and n-butanol extract content reaches up to more than 5.0%《Chinese Pharmacopoeia》2010
Legal index in year version one, it is possible to the effect of ensuring product compound Momordica grosvenori cough stopping tablet.
Embodiment
Below in conjunction with example, the invention will be further described:
Wherein, in following 1~embodiments of embodiment 3, the assay method of total alkaloid content is:Accurately weighed 10 grams of steps
The powder in C, add 70% ethanol 100ml to be heated to reflux 2 times, 1 hour every time, filtration, merging filtrate, be evaporated to obtain residue, add
Hydrochloric acid solution dissolves the residue, is transferred in 200ml volumetric flasks, adds hydrochloric acid solution to be settled to scale, shakes up, and filters, abandons
Primary filtrate is gone, then adds hydrochloric acid solution dissolving again, is transferred in another 200mL volumetric flask, adds hydrochloric acid solution to be settled to quarter
Degree;Precision measures subsequent filtrate 50ml, puts in separatory funnel, adjusts pH value to 9~10 with ammonia solution, shakes up, shaken with chloroform
Extraction 5 times, each 20ml is shaken, merges chloroform liquid, is washed with water 2 times, each 10ml, discards water lotion, chloroform liquid
Drying is put into the evaporating dish of constant weight, is evaporated, it is accurately weighed in 100 DEG C of dryings to constant weight, calculate, produce total alkaloid content.
The content assaying method of n-butanol extract is:Particle 3g described in step D is taken, it is finely ground, accurately weighed 2 grams, put
In 250ml boiling flasks, precision adds n-butanol 50ml, weighed weight, is heated to reflux 1 hour, lets cool, then weighed weight, uses
N-butanol supplies the weight of less loss, shakes up, and is filtered with dry filter paper;Primary filtrate is discarded, precision draws subsequent filtrate 25ml, puts and done
In the dry evaporating dish to constant weight, it is evaporated, is dried 3 hours at 105 DEG C, in dislocation drier, is cooled down 30 minutes, it is rapid accurately weighed
Weight, calculate, produce the content of n-butanol extract.
Embodiment 1
A kind of compound Momordica grosvenori cough stopping tablet, is prepared by the raw material of following parts by weight:Momordica grosvenori 562.5g, the root bark of white mulberry
150 g, the g of the tuber of stemona 375, the g of loguat leaf 2200, the g of Cynanchum glaucescens 225, the g of balloonflower root 137.5;
Its preparation method comprises the following steps:
A. above-mentioned parts by weight are pressed, Momordica grosvenori is added water to cook 4 times, decoction liquor is then combined with and filters, be finally concentrated into
Relative density is 1.20, obtains Momordica grosvenori clear cream;
B. above-mentioned weight fraction is pressed, the root bark of white mulberry, the tuber of stemona, loguat leaf, Cynanchum glaucescens, balloonflower root are added water to cook 2 times, will be decocted twice
Liquid merges, filtered, being concentrated into 1500mL, and the ethanol for then adding 4 times of amounts of concentrate stirs, and stands 48 hours, mistake
Filter, it is concentrated into the clear cream that relative density is 1.20;
C. the Momordica grosvenori clear cream that step A is obtained and the clear cream that step B is obtained are well mixed, dry, pulverize into powder, then
The powder is made to the particle of 20 mesh;
D. added in the particle that step C is obtained and account for the magnesium stearate of the granular mass 0.5% and account for the granular mass
0.5% talcum powder, it is well mixed, then carries out the detection of Determination of Total Alkaloid and n-butanol extract, measure finds every
The total alkaloid content of powder described in 0.51g is 0.9mg, measure find the n-butanol extract content of the particle for 5.3% its
In, the weight finally by every 0.68g is tabletted, and film coating obtains this compound Momordica grosvenori cough stopping tablet.
Embodiment 2
A kind of compound Momordica grosvenori cough stopping tablet, is prepared by the raw material of following parts by weight:Momordica grosvenori 562.5g, the root bark of white mulberry
150 g, the g of the tuber of stemona 375, the g of loguat leaf 2200, the g of Cynanchum glaucescens 225, the g of balloonflower root 137.5;
Its preparation method comprises the following steps:
A. above-mentioned parts by weight are pressed, Momordica grosvenori is added water to cook 4 times, decoction liquor is then combined with and filters, be finally concentrated into
Relative density is 1.20, obtains Momordica grosvenori clear cream;
B. above-mentioned weight fraction is pressed, the root bark of white mulberry, the tuber of stemona, loguat leaf, Cynanchum glaucescens, balloonflower root are added water to cook 2 times, will be decocted twice
Liquid merges, filtered, being concentrated into 1500mL, and the ethanol for then adding 4 times of amounts of concentrate stirs, and stands 48 hours, mistake
Filter, it is concentrated into the clear cream that relative density is 1.20;
C. the Momordica grosvenori clear cream that step A is obtained and the clear cream that step B is obtained are well mixed, dry, pulverize into powder, then
The powder is made to the particle of 22 mesh;
D. added in the particle that step C is obtained and account for the magnesium stearate of the granular mass 0.5% and account for the granular mass
0.5% talcum powder, it is well mixed, then carries out the detection of Determination of Total Alkaloid and n-butanol extract, measure finds every
The total alkaloid content of powder described in 0.51g is 1.3mg, measure find the n-butanol extract content of the particle for 4.9% its
In, the weight finally by every 0.60g is tabletted, and film coating obtains this compound Momordica grosvenori cough stopping tablet.
Embodiment 3
A kind of compound Momordica grosvenori cough stopping tablet, is prepared by the raw material of following parts by weight:Momordica grosvenori 562.5g, the root bark of white mulberry
150 g, the g of the tuber of stemona 375, the g of loguat leaf 2200, the g of Cynanchum glaucescens 225, the g of balloonflower root 137.5;
Its preparation method comprises the following steps:
A. above-mentioned parts by weight are pressed, Momordica grosvenori is added water to cook 4 times, decoction liquor is then combined with and filters, be finally concentrated into
Relative density is 1.20, obtains Momordica grosvenori clear cream;
B. above-mentioned weight fraction is pressed, the root bark of white mulberry, the tuber of stemona, loguat leaf, Cynanchum glaucescens, balloonflower root are added water to cook 2 times, will be decocted twice
Liquid merges, filtered, being concentrated into 1500mL, and the ethanol for then adding 4 times of amounts of concentrate stirs, and stands 48 hours, mistake
Filter, it is concentrated into the clear cream that relative density is 1.20;
C. the Momordica grosvenori clear cream that step A is obtained and the clear cream that step B is obtained are well mixed, dry, pulverize into powder, then
The powder is made to the particle of 20 mesh;
D. added in the particle that step C is obtained and account for the magnesium stearate of the granular mass 0.5% and account for the granular mass
0.5% talcum powder, it is well mixed, then carries out the detection of Determination of Total Alkaloid and n-butanol extract, measure finds every
The total alkaloid content of powder described in 0.51g is 1.3mg, measure find the n-butanol extract content of the particle for 5.3% its
In, the weight finally by every 0.51g is tabletted, and film coating obtains this compound Momordica grosvenori cough stopping tablet.
Product compound Momordica grosvenori cough stopping tablet made from 1~embodiment of embodiment 3 is subjected to quality testing, as a result such as table 1.
Table 1
As it can be seen from table 1 the legal items of pharmacopeia are fully achieved according to compound Momordica grosvenori cough stopping tablet produced by the present invention
Index, and indices show, it is its obtained compound Momordica grosvenori cough stopping tablet steady quality, controllable.
Claims (3)
- A kind of 1. compound Momordica grosvenori cough-relieving piece preparation method, it is characterised in that:This compound Momordica grosvenori cough stopping tablet is prepared by the raw material of following parts by weight:22.5 parts of Momordica grosvenori, 6 parts of the root bark of white mulberry, hundred 15 parts of portion, 88 parts of loguat leaf, 9 parts of Cynanchum glaucescens, 5.5 parts of balloonflower root;Its preparation method comprises the following steps:A. above-mentioned parts by weight are pressed, Momordica grosvenori is added water to cook 4 times, decoction liquor is then combined with and filters, are finally concentrated into relative Density is 1.20, obtains Momordica grosvenori clear cream;B. above-mentioned parts by weight are pressed, the root bark of white mulberry, the tuber of stemona, loguat leaf, Cynanchum glaucescens, balloonflower root are added water to cook 2 times, will decoction liquor twice Merge, filter, concentration, the ethanol for then adding 4 times of amounts of concentrate stir, and stand 48 hours, filtering, are concentrated into phase To the clear cream that density is 1.20;C. the Momordica grosvenori clear cream that step A is obtained and the clear cream that step B is obtained are well mixed, dry, pulverize into powder, then by institute State the particle that the mesh of 20 mesh~24 is made in powder;D. added in the particle that step C is obtained and account for the magnesium stearate of the granular mass 0.5% and account for the granular mass 0.5% Talcum powder, be well mixed, then carry out the detection of Determination of Total Alkaloid and n-butanol extract, it is last tabletted, Film coating obtains this compound Momordica grosvenori cough stopping tablet;Wherein, if found by measure per the total of particle described in 0.51g steps C Alkaloid is less than 5.0% less than the 1.0mg n-butanol extract contents for either finding the particle by measure, then exists The size of the compound Momordica grosvenori cough stopping tablet is adjusted during film-making so that the total alkaloid content of every compound Momordica grosvenori cough stopping tablet is not It is not less than 5.0% less than 1.0mg, n-butanol extract content;If found by measure per the total of particle described in 0.51g steps C Alkaloid finds that the n-butanol extract content of the particle is not less than 5.0% not less than 1.0mg and by measure, then not Need to adjust the size of the compound Momordica grosvenori cough stopping tablet in film-making, the weight according to every compound Momordica grosvenori cough stopping tablet is 0.51 gram of progress film-making.
- 2. a kind of compound Momordica grosvenori cough-relieving piece preparation method according to claim 1, it is characterised in that total described in step D Alkaloid content determination method is:The particle in accurately weighed 10 grams of step C, adds 70% ethanol 100ml to be heated to reflux 2 times, 1 hour every time, filtration, merging filtrate, it is evaporated to obtain residue, adds hydrochloric acid solution to dissolve the residue, be transferred to 200ml capacity In bottle, add hydrochloric acid solution to be settled to scale, shake up, filter, discard primary filtrate, then add hydrochloric acid solution dissolving again, be transferred to In another 200mL volumetric flask, hydrochloric acid solution is added to be settled to scale;Precision measures subsequent filtrate 50ml, puts in separatory funnel, uses ammonia Test solution adjusts pH value to 9~10, shakes up, with chloroform shaking extraction 5 times, each 20ml, merges chloroform liquid, be washed with water Wash 2 times, each 10ml, discard water lotion, chloroform liquid, which is put, to be dried into the evaporating dish of constant weight, is evaporated, is dried extremely at 100 DEG C Constant weight, it is accurately weighed, calculate, produce total alkaloid content.
- A kind of 3. compound Momordica grosvenori cough-relieving piece preparation method according to claim 1, it is characterised in that positive fourth described in step D The content assaying method of alcohol extracting thing is:Particle 3g described in step D is taken, it is finely ground, accurately weighed 2 grams, put 250ml boiling flasks In, precision adds n-butanol 50ml, weighed weight, is heated to reflux 1 hour, lets cool, then weighed weight, and less loss is supplied with n-butanol Weight, shake up, filtered with dry filter paper;Primary filtrate is discarded, precision draws subsequent filtrate 25ml, puts and dries to the evaporation of constant weight In ware, it is evaporated, is dried 3 hours at 105 DEG C, in dislocation drier, cooled down 30 minutes, rapid accurately weighed weight, calculates, produce The content of n-butanol extract.
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