CN100531714C - Preparing method of concentrated Shuanghuanglian oral liquid - Google Patents

Preparing method of concentrated Shuanghuanglian oral liquid Download PDF

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CN100531714C
CN100531714C CNB2003101102095A CN200310110209A CN100531714C CN 100531714 C CN100531714 C CN 100531714C CN B2003101102095 A CNB2003101102095 A CN B2003101102095A CN 200310110209 A CN200310110209 A CN 200310110209A CN 100531714 C CN100531714 C CN 100531714C
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add
ethanol
value
amount
filtrate
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CN1546095A (en
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邢泽田
李江华
张志平
姚静
陈进
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He'nan Zhulin Zhongsheng Pharmaceutical Industry Co Ltd
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He'nan Zhulin Zhongsheng Pharmaceutical Industry Co Ltd
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Abstract

The invention provides a process for preparing concentration type Shuanghuanglian oral liquid preparation, wherein the preparation comprises flower of honeysuckle, baikal skullcap root and capsule of weeping forsythia. The preparing process comprises acid deposition, alcohol deposition, pH adjustment, extraction, and high speed centrifuging.

Description

Be used to produce the preparation method of concentrated type SHUANGHUANGLIAN KOUFUYE
(1) technical field
The present invention relates to field of medicaments, is a kind of preparation method that is used to produce the concentrated type SHUANGHUANGLIAN KOUFUYE specifically.
(2) background technology
SHUANGHUANGLIAN KOUFUYE is antibiotic, the antiviral pure Chinese medicinal preparation of releasing in recent years.Has wind-dispelling heat-dissipating, the effect of eliminating fire and detoxication, removing heat from the lung and relieving sorethroat is applicable to bacillary and viral diseases such as heating that wind heat causes, upper respiratory tract infection, tonsillitis, pharyngitis, viral pneumonia, viral enteritis, bacterial enteritis, viral conjunctivitis, viral keratitis.Because the SHUANGHUANLIAN antibiosis and antiviral functions is remarkable, has filled up the shortage of clinical anti-bacteria and anti-virus medicine to a certain extent,, adopt SHUANGHUANLIAN also to receive curative effect preferably especially to not finding out the respiratory system infection of cause of disease as yet.And SHUANGHUANLIAN and multiple antibiotics medicine compatibility use the classic treatment scheme that has become treatment upper respiratory tract infection and various pneumonia.
As a kind of anti-bacteria and anti-virus preparation evident in efficacy, without any side effects, SHUANGHUANGLIAN KOUFUYE has obtained wideling popularize and has generally used.But adopt following preparation side to produce because existing SHUANGHUANGLIAN KOUFUYE---at first with behind the Radix Scutellariae decocting in water, acid precipitation, precipitate with ethanol, purification obtain Radix Scutellariae extract; Again with behind Flos Lonicerae, the Fructus Forsythiae decocting in water, concentrate, precipitate with ethanol, filtration obtain the Flos Lonicerae Fructus Forsythiae extract; Afterwards the said extracted thing is mixed, it is an amount of to add water, adjusts pH value, and cold preservation filters, and adds flavoring agent and makes oral liquid.Because existing preparation technology adopts traditional extraction, preparation method to realize, the extracts active ingredients of its medicine is incomplete, impurity content is higher, the extraction and application rate is low, cause concentration, the active constituent content of the oral liquid of producing low, to such an extent as to each oral consumption strengthens, and is not easy to take and carry.In addition, the increasing of dosage brings inconvenience such as pediatric patient also can for the crowd of the difficulty of taking medicine.
(3) summary of the invention
One object of the present invention provides a kind of oral liquid concentration and active constituent content and curative effect of can effectively improving more significant and can make it take, carry the preparation method that is used to produce the concentrated type SHUANGHUANGLIAN KOUFUYE more easily just at existing weak point in the above-mentioned existing preparation method.
The objective of the invention is to realize by following scheme:
The preparation method that is used to produce the concentrated type SHUANGHUANGLIAN KOUFUYE of the present invention is as follows:
This concentrated type SHUANGHUANGLIAN KOUFUYE is prepared from by weight by following component: wherein Radix Scutellariae 22~27%, Flos Lonicerae 22~27%, Fructus Forsythiae 47~53%.
Its preparation method comprises following processing step successively:
(a) Radix Scutellariae section back being added 8-10 times of water gaging decocted 1.5-2.5 hour, filter, medicinal residues add 5-6 times of water gaging again and decoct secondary, each 0.5-1 hour, filter, merge three times filtrate, filtrate concentrates and add hydrochloric acid solution in the time of 80 ℃ and regulates in right amount below the pH value to 3, is incubated 1 hour, and placement is spent the night, the bottom precipitation is added 6~8 times of water gagings to be stirred evenly, regulate pH value to 6-8 with 40% sodium hydroxide solution, add equivalent ethanol again, stir and make dissolving, filter, filtrate is regulated pH value to 1-3 with concentrated hydrochloric acid, places after 30 minutes 60 ℃ of insulations and spends the night, and filters, precipitation is washed till pH value 6-8 with ethanol, waves most ethanol and gets the Radix Scutellariae crude extract; Reuse 4-6 times of water gaging suspendible regulated pH value to 6-8, is stirred to dissolving, and add Radix Scutellariae crude extract amount 2-5% active carbon, stir, insulation more than 80 ℃ 30-40 minute, filter, filtrate adds dilute hydrochloric acid, and pH value transfers to 6-8, under agitation add equivalent 95% ethanol, sucking filtration transfers to 2-4 with hydrochloric acid, and 60 ℃ are incubated 30-40 minute, placement is spent the night, and obtains refining baicalin extract through draining.
(b) Flos Lonicerae, Fructus Forsythiae add 10-14 times of water gaging warm macerating after half an hour, are heated to boiling, and little boiling kept 1-2 hour, filter to get filtrate, and medicinal residues add 6-8 times of little the boiling of water gaging again and kept 1-1.5 hour, get filtrate, discard medicinal residues; Merge filtrate twice, evaporation and concentration to relative density is 1.20~1.25 (surveying under 70~80 ℃ of conditions), puts cold, under agitation slowly add ethanol, make to contain alcohol amount and reach 65-75%, put and leave standstill 24-48 hour in the cold room, the leaching supernatant, it is an amount of that residue adds ethanol, stirs evenly, and left standstill 24 hours, filter, merge ethanol liquid, recovery ethanol is not emitted after having the alcohol flavor, gets Flos Lonicerae, Fructus Forsythiae crude extract; A certain amount of n-butyl alcohol of reuse divides and extracts for 3-4 time, collects butanol extraction liquid, the reclaim under reduced pressure n-butyl alcohol, fine gold Flos Lonicerae, Fructus Forsythiae extract.
(c) will make with extra care baicalin extract, Flos Lonicerae, Fructus Forsythiae extract mixing by formula ratio, and it is an amount of to add water, is stirred to evenly, regulate pH value to 7-8 with 40% sodium hydroxide solution, stir evenly, place in the cold-storage jar, cold preservation is 72 hours under 4~8 ℃ of conditions, and afterwards by the remove impurity of high speed centrifugation mode, the sucrose that centrifugal liquid adds behind the dissolution filter is an amount of, stir, it is an amount of and regulate pH value to 6.5-7.5 to add essence again, adds water and makes total amount, fill, sterilization, promptly.
Because the present invention adopts modern separation, purification techniques when extracting effective ingredient, utilize methods such as different PH adjustings, n-butanol extraction, removes invalid impurity, and active constituent content is improved greatly, drug level increases.Moreover existing preparation method is after various extracts mix, and filters, leaves standstill, filters through filter stick, can not filter out impurities fully so on the one hand, has elongated the production cycle on the other hand, has increased cost consumption.And the present invention adopts high-speed centrifugation technology, not only to greatest extent filtering impurity, and need not leave standstill after centrifugal, directly fill has been shortened the production cycle greatly, has reduced production cost.
The present invention compares with existing preparation method, and its advantage is: active constituent content is improved, and is the twice of original same dose, and valid density has increased by one times in the unit volume, and the production cycle shortens the corresponding production cost that reduced to some extent.Again because active constituent content improves, valid density increases in the unit volume, the corresponding minimizing of its oral consumption, make take, carry more convenient; Particularly, provide convenience to the child patient of the comparison difficulty of taking medicine.
(4) specific embodiments
The present invention is described further below in conjunction with embodiment, but does not limit the present invention.
Example 1:
(a) get Radix Scutellariae section 750g and add 10 times of water gagings decoctions 2 hours, filter, medicinal residues add 6 times of water gagings again and decoct secondary, each 1 hour, filter, merge three times filtrate, filtrate concentrates and add hydrochloric acid solution in the time of 80 ℃ regulates pH value to 2.0 in right amount, is incubated 1 hour, and placement is spent the night, the bottom precipitation is added 8 times of water gagings to be stirred evenly, regulate pH value to 7.0 with 40% sodium hydroxide solution, add equivalent ethanol again, stir and make dissolving, filter, filtrate is regulated pH value to 2.0 with concentrated hydrochloric acid, places after 30 minutes 60 ℃ of insulations and spends the night, and filters, precipitation is washed till pH value to 7.0 with ethanol, waves most ethanol and gets the Radix Scutellariae crude extract; 6 times of water gaging suspendibles of reuse are regulated pH value to 7.0, are stirred to dissolving, and add Radix Scutellariae crude extract amount 3% active carbon, stir, insulation more than 80 ℃ 30 minutes, filter, filtrate adds dilute hydrochloric acid, and pH value transfers to 7, under agitation add equivalent 95% ethanol, sucking filtration transfers to 2.8,60 ℃ of insulations 30 minutes with hydrochloric acid, placement is spent the night, and obtains refining baicalin extract through draining.
(b) extracting honeysuckle 750g, Fructus Forsythiae 1500g add 12 times of water gaging warm macerating after half an hour, are heated to boiling, and little boiling kept 1.5 hours, filter to get filtrate, and medicinal residues add 8 times of little boiling of water gaging again and kept 1.5 hours, get filtrate, discard medicinal residues; Merge filtrate twice, evaporation and concentration to relative density is 1.21 (surveying under 80 ℃ of conditions), puts cold, under agitation slowly add ethanol, make to contain alcohol amount and reach 70%, put and leave standstill 24 hours in the cold room, the leaching supernatant, it is an amount of that residue adds ethanol, stirs evenly, and left standstill 24 hours, filter, merge ethanol liquid, recovery ethanol is not emitted after having the alcohol flavor, gets Flos Lonicerae, Fructus Forsythiae crude extract; A certain amount of n-butyl alcohol of reuse divides and extracts for 4 times, the filtering extract, the reclaim under reduced pressure n-butyl alcohol, fine gold Flos Lonicerae, Fructus Forsythiae extract.
(c) above-mentioned refining baicalin extract, Flos Lonicerae, Fructus Forsythiae extract are mixed, and it is an amount of to add water, is stirred to evenly, regulate pH value to 7.5 with 40% sodium hydroxide solution, stir evenly, cold preservation (under 6 ℃ of conditions) is 72 hours in the cold-storage jar, adopt ultracentrifugal mode to carry out remove impurity, centrifugal liquid adds the sucrose (300g) behind the dissolution filter, stirs, and it is an amount of and regulate pH value to 7.0 to add essence again, add water and make 1000ml, fill, sterilization, promptly.
Embodiment 2:
(a) get Radix Scutellariae section 750g and add 9 times of water gagings decoctions 1 hour 50 minutes, filter, medicinal residues add 5.5 times of water gagings again and decoct secondary, each 50 minutes, filter, merge three times filtrate, filtrate concentrates and add hydrochloric acid solution in the time of 80 ℃ regulates pH value to 2.5 in right amount, is incubated 1 hour, and placement is spent the night, the bottom precipitation is added 7 times of water gagings to be stirred evenly, regulate pH value to 7.5 with 40% sodium hydroxide solution, add equivalent ethanol again, stir and make dissolving, filter, filtrate is regulated pH value to 2.5 with concentrated hydrochloric acid, places after 30 minutes 60 ℃ of insulations and spends the night, and filters, precipitation is washed till pH value to 7.5 with ethanol, waves most ethanol and gets the Radix Scutellariae crude extract; 5 times of water gaging suspendibles of reuse are regulated pH value to 7.5, are stirred to dissolving, and add Radix Scutellariae crude extract amount 4% active carbon, stir, insulation more than 80 ℃ 35 minutes, filter, filtrate adds dilute hydrochloric acid, and pH value transfers to 7.5, under agitation add equivalent 95% ethanol, sucking filtration transfers to 3,60 ℃ of insulations 30 minutes with hydrochloric acid, placement is spent the night, and obtains refining baicalin extract through draining.
(b) extracting honeysuckle 750g, Fructus Forsythiae 1500g add 13 times of water gaging warm macerating after half an hour, are heated to boiling, and little boiling kept 1 hour 50 minutes, filter to get filtrate, and medicinal residues add 7 times of little boiling of water gaging again and kept 1.5 hours, get filtrate, discard medicinal residues; Merge filtrate twice, evaporation and concentration to relative density is 1.24 (surveying under 75 ℃ of conditions), puts cold, under agitation slowly add ethanol, make to contain alcohol amount and reach 75%, put and leave standstill 36 hours in the cold room, the leaching supernatant, it is an amount of that residue adds ethanol, stirs evenly, and left standstill 24 hours, filter, merge ethanol liquid, recovery ethanol is not emitted after having the alcohol flavor, gets Flos Lonicerae, Fructus Forsythiae crude extract; A certain amount of n-butyl alcohol of reuse divides and extracts for 4 times, the filtering extract, the reclaim under reduced pressure n-butyl alcohol, fine gold Flos Lonicerae, Fructus Forsythiae extract.
(c) above-mentioned refining baicalin extract, Flos Lonicerae, Fructus Forsythiae extract are mixed, and it is an amount of to add water, is stirred to evenly, regulate pH value to 7.8 with 40% sodium hydroxide solution, stir evenly, cold preservation (under 5 ℃ of conditions) is 72 hours in the cold-storage jar, adopt ultracentrifugal mode to carry out remove impurity, centrifugal liquid adds the sucrose (300g) behind the dissolution filter, stirs, and it is an amount of and regulate pH value to 7.5 to add essence again, add water and make 1000ml, fill, sterilization, promptly.

Claims (1)

1, a kind of preparation method that is used to produce the concentrated type SHUANGHUANGLIAN KOUFUYE, it is characterized in that: it comprises following processing step successively:
(a) Radix Scutellariae is cut into slices 750g adds 8-10 times of water gaging and decocted 1.5-2.5 hour, filter, medicinal residues add 5-6 times of water gaging again and decoct secondary, each 0.5-1 hour, filter, merge three times filtrate, filtrate concentrates and add hydrochloric acid solution in the time of 80 ℃ and regulates in right amount below the pH value to 3, is incubated 1 hour, and placement is spent the night, the bottom precipitation is added 6~8 times of water gagings to be stirred evenly, regulate pH value to 6-8 with 40% sodium hydroxide solution, add equivalent ethanol again, stir and make dissolving, filter, filtrate is regulated pH value to 1-3 with concentrated hydrochloric acid, places after 30 minutes 60 ℃ of insulations and spends the night, and filters, precipitation is washed till pH value 6-8 with ethanol, waves most ethanol and gets the Radix Scutellariae crude extract; Reuse 4-6 times of water gaging suspendible regulated pH value to 6-8, is stirred to dissolving, and add Radix Scutellariae crude extract amount 2-5% active carbon, stir, insulation more than 80 ℃ 30-40 minute, filter, filtrate adds dilute hydrochloric acid, and pH value transfers to 6-8, under agitation add equivalent 95% ethanol, sucking filtration transfers to 2-4 with hydrochloric acid, and 60 ℃ are incubated 30-40 minute, placement is spent the night, and obtains refining baicalin extract through draining;
(b) extracting honeysuckle 750g, Fructus Forsythiae 1500g add 10-14 times of water gaging warm macerating after half an hour, are heated to boiling, and little boiling kept 1-2 hour, filter to get filtrate, and medicinal residues add 6-8 times of little the boiling of water gaging again and kept 1-1.5 hour, get filtrate, discard medicinal residues; Merge filtrate twice, evaporation and concentration to relative density is 1.20~1.25, and this relative density should record under 70~80 ℃ of conditions, put cold after, under agitation slowly add ethanol, make the alcohol amount of containing reach 65-75%, put and leave standstill 24-48 hour in the cold room, the leaching supernatant, it is an amount of that residue adds ethanol, stir evenly, left standstill 24 hours, and filtered, merge ethanol liquid, recovery ethanol is not emitted after having the alcohol flavor, gets Flos Lonicerae, Fructus Forsythiae crude extract; A certain amount of n-butyl alcohol of reuse divides and extracts for 3-4 time, collects butanol extraction liquid, the reclaim under reduced pressure n-butyl alcohol, fine gold Flos Lonicerae, Fructus Forsythiae extract;
(c) the refining baicalin extract that step a step b is made, Flos Lonicerae, Fructus Forsythiae extract mix, and it is an amount of to add water, are stirred to evenly, regulate pH value to 7-8 with 40% sodium hydroxide solution, stir evenly, place in the cold-storage jar, cold preservation is 72 hours under 4~8 ℃ of conditions, and afterwards by the remove impurity of high speed centrifugation mode, the sucrose that centrifugal liquid adds behind the dissolution filter is an amount of, stir, it is an amount of and regulate pH value to 6.5-7.5 to add essence again, adds water and makes 1000ml total amount, fill, sterilization, promptly.
CNB2003101102095A 2003-12-09 2003-12-09 Preparing method of concentrated Shuanghuanglian oral liquid Expired - Lifetime CN100531714C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102266386A (en) * 2010-06-01 2011-12-07 四川大千药业有限公司 Scutellaria baicalensis extract and preparation method and uses thereof

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102349944B (en) * 2010-06-01 2014-05-07 四川大千药业有限公司 Nasal thermosensitive in-situ gel prepared by radix scutellariae extract, its preparation method and its application
CN102266567B (en) * 2010-06-01 2013-01-02 四川大千药业有限公司 Radix scutellariae extractive phospholipid complex, and preparation method and purpose thereof
CN103961412B (en) * 2014-01-22 2017-01-18 深圳市瑞莱贵生生物医药科技有限公司 Traditional Chinese medicine composition as well as preparation method and application thereof
CN111568952A (en) * 2020-05-18 2020-08-25 四川省欧邦动物药业有限公司 Concentrated Shuanghuanglian oral liquid preparation for production and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102266386A (en) * 2010-06-01 2011-12-07 四川大千药业有限公司 Scutellaria baicalensis extract and preparation method and uses thereof
CN102266386B (en) * 2010-06-01 2013-05-01 四川大千药业有限公司 Scutellaria baicalensis extract and preparation method and uses thereof

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