CN101254226B - Duliang compound chinese medicine soft capsules - Google Patents

Duliang compound chinese medicine soft capsules Download PDF

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CN101254226B
CN101254226B CN2007100931643A CN200710093164A CN101254226B CN 101254226 B CN101254226 B CN 101254226B CN 2007100931643 A CN2007100931643 A CN 2007100931643A CN 200710093164 A CN200710093164 A CN 200710093164A CN 101254226 B CN101254226 B CN 101254226B
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CN101254226A (en
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刘小英
陈烈春
石锦萍
王道权
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Chongqing Huasen Pharmaceutical Co ltd
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游洪涛
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Abstract

The invention discloses a Duliang compound soft capsule and a preparation method thereof. The soft capsule comprises the following components (per 1,000 capsules) angelica dahurica 1,128 g, ligusticum chuanxiong 282 g, and soybean oil 324-432 g. The preparation method comprises the following steps of extracting angelica dahurica and ligusticum chuanxiong with supercritical carbon dioxide to obtain volatile oil and residue; decocting the residue in water, precipitating with ethanol, vacuum drying at low temperature, and making into soft capsule. The soft capsule uses soft capsule shell material to wrap medicinal content, so as to mask the bitter taste and unpleasant taste of the medicinal content. The inventive soft capsule also has the advantages of easy administration, rapid release of medicinal content after disintegration of the soft capsule shell material, quick action, remarkably increased content of active ingredients such as imperatorin by using supercritical carbon dioxide extraction technique, high bioavailability of medicinal content, reduced impurities of extract powder, more accurately dosage, remarkably reduced particle size of medicinal powder, quick absorption during clinical treatment, good therapeutic effect, and no toxic or side effects.

Description

A kind of all beams herbal mixture soft capsule
Technical field
The present invention relates to a kind of migrainous Chinese medicine composition and preparation technology thereof of being used for the treatment of, relate in particular to DULIANG RUANJIAONANG and preparation technology thereof.
Background technology
All the beam ball starts from Song dynasty king CHYOU " 101 choosing side ", is a classics recipe, its mainly by the Radix Angelicae Dahuricae and Rhizoma Chuanxiong by a certain percentage compatibility form, Radix Angelicae Dahuricae root acrid in the mouth is and warm in nature, it is a kind of plant that acts on stomach, large intestine, pulmonary.But pungent plant blood stasis dispelling and regulating the flow of vital energy, so Radix Angelicae Dahuricae root has the ability of removing wind and cold in the head.The Rhizoma Chuanxiong rhizome also is an acrid in the mouth and warm in nature, but it is to act on liver, gallbladder and heart week, and it has circulation of the QI and blood of lifting and lenitive function.Modern pharmacy studies show that: Radix Angelicae Dahuricae root has compositions such as imperatorin, isoimperatorin, angelicin, Radix Angelicae Dahuricae ethers, and these compositions are alleviating pains, make excited calm, the main effective ingredient that prevents and reduce inflammation.The Rhizoma Chuanxiong rhizome has lactone and many phenols such as compositions such as alkaloid and ferulic acid, and these compositions are to invigorate blood circulation and the main effective ingredient of analgesic.Nasal obstruction and headache a kind ofly are easy to take place in winter in spring, and caused that by wind and cold the paathogenic factor of common disease headache is: ailment said due to cold or exposure and cold-evil act on head, cause that tangible yang-energy can not normal circulation, QI and blood stagnation and head path blockade.If wind and cold acts on lung, then lung can not eupnea, and gas can not trouble-free operation in the lung, then causes nasal obstruction, and therefore all beam is suitable for expelling wind and cold, promoting blood circulation to remove obstruction in the collateral, and it is obstructed to be used for the treatment of the nasal obstruction that heresy of wind and cold cause, migraine and general headache, or accompany the cold and heat disease, curative effect is better.All beams ball of Chinese medicine production technology preparation is to soak the Radix Angelicae Dahuricae after the steaming, Rhizoma Chuanxiong with a certain proportion of yellow wine by prescription, to be ground into fine powder, to sieve, and mixing adds refined honey, makes big honeyed pills.But there is thick, big, black problem in all beams ball of making like this, and quality of production poor stability, and curative effect is unsecured, is difficult to when patient takes accept, and is restricted in clinical use.For addressing the aforementioned drawbacks, all beams drop pill of prior art has improved traditional preparation technology, at present commercially available all beams drop pill is after a certain amount of extract solid or liquid medicine and substrate such as Polyethylene Glycol or other medicinal materials heat fused are mixed, splash in the not miscible condensed fluid, the preparation that shrinks condensation and make, all the production of beam drop pill employing pharmaceutic adjuvant such as Polyethylene Glycol are more, thereby active constituent content will hang down relatively, its active ingredient underdosage, clinical efficacy is relatively poor; And all the beam drop pill is after ingredient and adjuvant Polyethylene Glycol heat fused are mixed, splash in the not miscible condensed fluid, the preparation that shrinks condensation and make, therefore the part medicine is to be exposed to the pill surface, so the drop pill medicine stability is undesirable, and bitterness and the abnormal flavour aspect of covering the drug substance contents discomfort are also bad, and owing to the stimulation of bitterness and abnormal flavour, nausea easily caused nausea when the patient took this drop pill.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of all beams herbal mixture soft capsule.For realizing purpose of the present invention, a kind of all beams herbal mixture soft capsule of the present invention contains following ingredients: the Radix Angelicae Dahuricae: 1128g, Rhizoma Chuanxiong: 282g, soybean oil: 324-432g in per 1000 soft capsules.
Further, the shell of described soft capsule contains opacifier;
Further, described opacifier is Fe 2O 3And Fe 3O 4Mixture.
Another object of the present invention is to provide the technology of the above-mentioned all beams herbal mixture soft capsule of preparation, may further comprise the steps:
A. the CO of effective ingredient 2Supercritical extraction
Press prescription, after the Radix Angelicae Dahuricae, the Rhizoma Chuanxiong that cooks mixed, mixture is carried out carbon dioxide supercritical fluid extraction under cryogenic conditions, process conditions: extraction temperature: 30-60 ℃, extracting pressure: 15-30Mpa, extraction time: 2-5 hour, CO 2Flow: 300~350L/h gets mixture volatile oil, medicinal residues, collects stand-by respectively;
B. the water boiling and extraction of medicinal residues
The medicinal residues of step a are added 8~10 times of amounts of water, and heating is boiled and is carried 5 hours after-filtration under normal pressure, and the filtrate that will contain effective ingredient concentrates, and measures in the time of 60 ℃, and proportion is the thick paste of 1.03~1.07g/ml, collects stand-by;
C. precipitate with ethanol
The thick paste of step b is stirred the ethanol that adds 6 times of amounts, leave standstill 24 hours after-filtration, collect filtrate, reclaim ethanol, concentrated filtrate is measured in the time of 60 ℃, and proportion is the thick paste of 1.03~1.07g/ml, collects stand-by;
D. low-temperature vacuum drying
Starch is an amount of with adding in the thick paste of step c gained, gets drug extract, and this extractum turns round vacuum drying through low-temperature microwave, drying condition: 70~80 ℃ of temperature, and pressure-0.07~0.08Mpa gets the medicine dry extract 2~3 hours drying times, and is stand-by;
E. micronizing
With the dried cream powder that steps d obtains, pulverize process conditions: air consumption 40M with super micron mill 3/ min, operating pressure 0.75Mpa gets particle diameter and is 0.5~15 μ m fine powder, and is stand-by;
F. suppress capsule
The volatile oil of step a gained mixed with step e gained extract powder and add soybean oil, be pressed into capsule after fully mixing by prescription, after the cold drying finished product.
The invention has the beneficial effects as follows, use the soft capsule packaging medicine, the bitterness and the abnormal flavour of drug substance contents discomfort have been covered, solve the Radix Angelicae Dahuricae, Rhizoma Chuanxiong extract and made us the problem that is difficult to take, swallow easily, soft capsule is once disintegrate, and content just together discharges immediately, so it is produce effects is rapid, better than the obviously fast also absorption of pill, drop pill; The medicine stability height.Because some easy oxidation in the Radix Angelicae Dahuricae Rhizoma Chuanxiong extract, meet effective ingredient imperatorin in the damp and hot unsettled ingredient such as the Radix Angelicae Dahuricae etc., it is prepared into the capsule of sealing, and interpolation opacifier, be subjected to the effect of oxygen, light in wet and the air with protection medicine, thereby improved this stability of drug.Adopt process of the present invention, effective ingredient such as imperatorin have been brought up to every 0.32mg by every 0.16mg of traditional handicraft, have reduced the impurity of extract powder, and dosage is more accurate relatively, and degree of accuracy is higher, can reach the metering of milligram/grain; The bioavailability of medicament height.And because the particle diameter of drug powder reduces greatly, absorb soon when being used for clinical treatment, good effect has no side effect.
Other advantage of the present invention, target and feature will be set forth to a certain extent in the following description, and to a certain extent, based on being conspicuous to those skilled in the art, perhaps can obtain instruction from the practice of the present invention to investigating hereinafter.
Description of drawings
The present invention is described in further detail below in conjunction with accompanying drawing.
Fig. 1 is the process chart of extracts active ingredients of the present invention;
Fig. 2 is a capsule granulating process flow chart of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail, rather than restriction the present invention.
Embodiment 1 prepares 1000 beam compound capsules
Technological process as shown in Figure 1, 2 prepares according to following step:
A. the CO of effective ingredient 2Supercritical extraction
By prescription, after Radix Angelicae Dahuricae 1128g, the Rhizoma Chuanxiong 282g mixing that cooks, mixture is carried out cryogenic conditions carbon dioxide supercritical extraction, process conditions: extraction temperature: 30 ℃, extracting pressure: 15Mpa, the extraction time: 2 hours, CO 2Flow 300L/h gets mixture volatile oil, medicinal residues, collects stand-by;
B. the water boiling and extraction of medicinal residues
The medicinal residues of step a are added 8 times of amounts of water, and heating is boiled and is carried 5 hours after-filtration under normal pressure, and the filtrate that will contain effective ingredient concentrates, and measuring to proportion in the time of 60 ℃ is the thick paste of 1.03g/ml, collects stand-by;
C. precipitate with ethanol
The thick paste of step b is stirred the ethanol that adds 6 times of amounts, leave standstill 24 hours after-filtration, collect filtrate, reclaim ethanol, filtrate is concentrated, measuring to proportion in the time of 60 ℃ is the thick paste of 1.03g/ml, collects stand-by;
D. low-temperature vacuum drying
Starch is an amount of with adding in the thick paste of step c gained, gets drug extract, and this extractum turns round vacuum drying through low-temperature microwave, drying condition: 70 ℃ of temperature, and pressure-0.07Mpa gets the medicine dry extract 2~3 hours drying times, and is stand-by;
E. micronizing
With the dried cream powder that steps d obtains, pulverize process conditions: air consumption 40M with super micron mill 3/ min, operating pressure 0.75Mpa gets particle diameter and is 0.5~15 μ m fine powder, and is stand-by;
F. suppress capsule
The volatile oil of step a gained mixed with step e gained extract powder and add soybean oil 380g, be pressed into 1000 capsules after fully mixing by prescription, after the cold drying finished product.
Embodiment 2
Technological process as shown in Figure 1, 2 prepares according to following step:
A.CO 2Supercritical extraction
By prescription, after Radix Angelicae Dahuricae 1128g, the Rhizoma Chuanxiong 282g mixing that cooks, mixture is carried out cryogenic conditions carbon dioxide supercritical extraction, process conditions: extraction temperature: 45 ℃, extracting pressure: 20Mpa, extraction time: 4 hours; CO 2Flow 320L/h gets mixture volatile oil, medicinal liquid, medicinal residues, and volatile oil is waited to collect stand-by;
B. the water boiling and extraction of medicinal residues
The medicinal residues of step a are added 9 times of amounts of water, and heating is boiled and is carried 5 hours after-filtration under normal pressure, and the filtrate that will contain effective ingredient concentrates, and measures in the time of 60 ℃, and proportion is the thick paste of 1.05g/ml, collects stand-by;
C. precipitate with ethanol
The thick paste of step b is stirred the ethanol that adds 6 times of amounts, leave standstill 24 hours after-filtration, collect filtrate, reclaim ethanol, filtrate is concentrated, measuring to proportion in the time of 60 ℃ is the thick paste of 1.05g/ml, collects stand-by;
D. low-temperature vacuum drying
Starch is an amount of with adding in the thick paste of step c gained, gets drug extract, and this extractum turns round vacuum drying through low-temperature microwave, drying condition: 70 ℃ of temperature, and pressure 0.01Mpa gets the medicine dry extract 2.5 hours drying times, and is stand-by;
E. micronizing
With the dried cream powder that steps d obtains, pulverize process conditions: air consumption 40M with super micron mill 3/ min, operating pressure 0.75Mpa gets particle diameter and is 0.5~15 μ m fine powder, and is stand-by;
F. suppress capsule
The volatile oil of step a gained mixed with step e gained extract powder and add soybean oil 380g, be pressed into 1000 capsules after fully mixing by prescription, after the cold drying finished product.
Embodiment 3
Technological process as shown in Figure 1, 2 prepares according to following step:
A.CO 2Supercritical extraction
By prescription, after Radix Angelicae Dahuricae 1128g, the Rhizoma Chuanxiong 282g mixing that cooks, mixture is carried out cryogenic conditions carbon dioxide supercritical extraction, process conditions: extraction temperature: 60 ℃, extracting pressure: 30Mpa, the extraction time: 5 hours, CO 2Flow: 350L/h gets mixture volatile oil, medicinal liquid, medicinal residues, and volatile oil is waited to collect stand-by;
B. the water boiling and extraction of medicinal residues
The medicinal residues of step a are added 10 times of amounts of water, and heating is boiled and is carried 5 hours after-filtration under normal pressure, and the filtrate that will contain effective ingredient concentrates, and measures in the time of 60 ℃, and proportion is the thick paste of 1.07g/ml, collects stand-by;
C. precipitate with ethanol
The thick paste of step b is stirred the ethanol that adds 6 times of amounts, leave standstill 24 hours after-filtration, collect filtrate, reclaim ethanol, filtrate is concentrated, measuring to proportion in the time of 60 ℃ is the thick paste of 1.07g/ml, collects stand-by;
D. low-temperature vacuum drying
Starch is an amount of with adding in the thick paste of step c gained, gets drug extract, and this extractum turns round vacuum drying through low-temperature microwave, drying condition: 80 ℃ of temperature, and pressure 0.08Mpa gets the medicine dry extract 3 hours drying times, and is stand-by;
E. micronizing
With the dried cream powder that steps d obtains, pulverize process conditions: air consumption 40M with super micron mill 3/ min, operating pressure 0.75Mpa gets particle diameter and is 0.5~15 μ m fine powder, and is stand-by;
F. suppress capsule
The volatile oil of step a gained mixed with steps d gained extract powder and add soybean oil 432g, be pressed into capsule after fully mixing by prescription, after the cold drying finished product.
Effect experiment:
All beams preparation of the inventive method preparation can alleviate Oleum Tiglii induced mice ear swelling, shows antiinflammatory action; Can improve mice to physics and the pain caused threshold value of chemical factor, show analgesic activity; Clinical research is the result show, it is the headache disease that a variety of causes causes that all beams preparation of the inventive method preparation adapts to disease, and especially headache belongs to wind and cold stagnation of blood stasis venation card person, disease is seen distending pain in the head or twinge, localized pain, outbreak repeatedly meets that wind and cold brings out or the person of increasing the weight of is better.
Contrast test:
Viewing test case 418 examples, contrast case 156 examples.Clinical experimental study is the result show: test group treatment headache recovery from illness case 146, recovery from illness case rate 34.93%; Produce effects case 172 examples, produce effects case rate 41.15%; Effective case 80 examples, effectively case rate 19.14%; Total effective rate reaches 95.22%.Treatment of control group headache recovery from illness case 14, recovery from illness case rate 8.97%; Produce effects case 25 examples, produce effects case rate 16.03%; Effective case 43 examples, effectively case rate 27.56%; Total effective rate is 52.56%.Two groups of curative effects relatively have significant differences, and investigational agent significantly is better than contrasting medicine.Duration of test, medicine does not have obvious influence to blood, urine, stool routine examination, the heart, liver, renal function, does not see obvious adverse reaction.Therefore the clinical practice of the DULIANG RUANJIAONANG of the inventive method preparation is safely and effectively.
Above-mentioned experimental result shows, adopts the pill drop pill and the ratio of DULIANG RUANJIAONANG with the prior art of preparation technology's preparation of the present invention, has the bioavailability height, it is the effective component content height of same units preparation, disintegration rate is fast, the advantage that onset time is short, and medicine stability is good.
Although by reference some preferred embodiment of the present invention, invention has been described, but those of ordinary skill in the art is to be understood that, can make various changes to it in the form and details, and the spirit and scope of the present invention that do not depart from appended claims and limited.

Claims (3)

1. beam compound capsules all, it is characterized in that: per 1000 soft capsules are mainly made by following raw material: the Radix Angelicae Dahuricae: 1128g, Rhizoma Chuanxiong: 282g, soybean oil: 324~432g;
Its preparation technology may further comprise the steps:
A. the CO of effective ingredient 2Supercritical extraction:
Press prescription, after the Radix Angelicae Dahuricae, the Rhizoma Chuanxiong that cooks mixed, mixture is carried out carbon dioxide supercritical fluid extraction under cryogenic conditions, process conditions: extraction temperature: 30~60 ℃, extracting pressure: 15~30Mpa, the extraction time: 2~5 hours, CO 2Flow: 300~350L/h obtains mixture volatile oil, medicinal residues, and collects stand-by respectively;
B. the water boiling and extraction of medicinal residues
The medicinal residues of step a are added 8~10 times of amounts of water, and heating is boiled and is carried 5 hours after-filtration under normal pressure, measures when temperature is 60 ℃, and the filtrate that will contain effective ingredient is concentrated into the thick paste that proportion is 1.03~1.07g/ml, collects stand-by;
C. precipitate with ethanol
The thick paste of step b is stirred the ethanol that adds 6 times of amounts, leave standstill 24 hours after-filtration, collect filtrate, reclaim ethanol, when temperature is 60 ℃, measure, filtrate is concentrated into the thick paste that proportion is 1.03~1.07g/ml, collect stand-by;
D. low-temperature vacuum drying
Starch is an amount of with adding in the thick paste of step c gained, gets drug extract, and this extractum turns round vacuum drying through low-temperature microwave, drying condition: 70~80 ℃ of temperature, and pressure-0.07~0.08Mpa gets the medicine dry extract 2~3 hours drying times, and is stand-by;
E. micronizing
With the dried cream powder that steps d obtains, pulverize process conditions: air consumption 40M with super micron mill 3/ min, operating pressure 0.75Mpa gets particle diameter and is 0.5~15 μ m fine powder, and is stand-by;
F. suppress capsule
The volatile oil of step a gained mixed with step e gained extract powder and add soybean oil, be pressed into capsule after fully mixing by prescription, after the cold drying finished product.
2. all beams compound capsules according to claim 1, it is characterized in that: the shell of described soft capsule contains opacifier.
3. all beams compound capsules according to claim 2 is characterized in that: described opacifier is Fe 2O 3And Fe 3O 4Mixture.
CN2007100931643A 2007-12-19 2007-12-19 Duliang compound chinese medicine soft capsules Active CN101254226B (en)

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102048764B (en) * 2009-11-05 2015-05-13 天津天士力现代中药资源有限公司 Use of microwave drying technique in field of traditional Chinese medicinal extract
CN103449533B (en) * 2012-05-29 2015-02-18 华东理工大学 Supercritical carbon dioxide method for extraction separation of magnetosomes from magnetotactic bacteria
CN102772459A (en) * 2012-08-14 2012-11-14 中山大学 In-situ gel for treating migraine and preparation method thereof
EP3466930B1 (en) 2013-02-08 2022-07-20 General Mills, Inc. Reduced sodium food product
CN108567753A (en) * 2017-06-08 2018-09-25 北京九龙制药有限公司 All beam dripping pill and its preparation process

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
袁媛等.中药复方制剂制备工艺中挥发油取舍问题探讨.《热带药学》.2007,(第1期),83-85. *

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