CN103977071A - Clinopodium polycephalum tablet and preparation method thereof - Google Patents
Clinopodium polycephalum tablet and preparation method thereof Download PDFInfo
- Publication number
- CN103977071A CN103977071A CN201410247510.9A CN201410247510A CN103977071A CN 103977071 A CN103977071 A CN 103977071A CN 201410247510 A CN201410247510 A CN 201410247510A CN 103977071 A CN103977071 A CN 103977071A
- Authority
- CN
- China
- Prior art keywords
- extraction
- herba clinopodii
- supercritical
- extract
- tabellae
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a clinopodium polycephalum tablet and a preparation method thereof. The preparation method comprises the following concrete steps: grinding clinopodium polycephalum at the temperature of 10 DEG C, and sieving through a 10-mesh sieve; extracting the sieved clinopodium polycephalum powder in a supercritical CO2 extracting device under conditions that the extraction temperature is 25 DEG C, the extraction pressure is 20MPa, the flow rate of CO2 is 2L/h, wherein the extracting manner is combination of dynamic extraction and static extraction, particularly the static extraction is carried out for 10-15 minutes firstly and then the dynamic extraction is carried out for 5-10 minutes, one-time dynamic extraction and one-time static extraction are taken as an extraction cycle, the cycle is carried out twice, 1.2ml/g of absolute ethanol and 0.08g/g of N2 acyl lysine (based on the total amount of the clinopodium polycephalum) is added during the extraction; performing two-stage separation after the extraction is completed under the conditions that the separation temperature is 25 DEG C and the separation pressure is 5MPa; and recycling the ethanol from the separated extracted solution to obtain an extract for later use; taking 1 part of clinopodium polycephalum supercritical CO2 fluid extract, 32 parts of microcrystalline cellulose, 38 parts of cross-linked sodium carboxymethylcellulose, 16 parts of processing agar, 6 parts of protein sugar and 7 parts of lactose, and pressing into tablets by adopting a conventional method.
Description
Technical field
The present invention relates to one Herba Clinopodii Tabellae, tablet for cooling blood and relieving pain of specifically making taking Herba Clinopodii as raw material and preparation method thereof.
Background technology
Herba Clinopodii Tabellae is made up of the extract of the Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali) (clinopodium polyeephalum) or Herba Clinopodii Polycephali (Clinopodium chinese).Former plant is hemorrhage among the people.Research in recent years and clinically all prove, this medicine has significant anastalsis to multiple hemorrhage, is mainly applicable to dysfunctional uterine hemorrhage, menorrhagia, postpartum hemorrhage, hematuria and nose and the disease such as looks.
After autotomying and doubly finding the seventies in last century and record, its active component, control effect and mechanism and preparation type are carried out to research for many years.The beginning of the nineties in last century, " Chinese Pharmacopoeia. one " record this medicine, medicine name Herba Clinopodii in (1990) newly-increased kind.In the medicinal plants Herba Clinopodii Polycephali and the Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali) of Chinese medicine Herba Clinopodii, contain saponins, flavonoid, amino acids, polysaccharide, phenolic substance and volatilization wet goods compound, wherein saponins and flavone compound are the effective ingredient of Herba Clinopodii hemostasis, antiinflammatory.
Herba Clinopodii wide material sources, all there is product all parts of the country, for convenience of clinical application, the nineties existing Herba Clinopodii Tabellae be written into " Chinese Pharmacopoeia. one " (1990) as standardized drug, there are successively the different dosage forms such as Herba Clinopodii oral liquid, Herba Clinopodii capsule, Herba Clinopodii granule to appear on the market later, clinical use is more and more extensive, is usually used in the aspects such as hemostatic analgesia antiinflammatory, and curative effect is original.Modern pharmacology experiment show its mainly have hemostasis, antibacterial, reduce blood pressure, shrink the multiple biological activitys such as uterine function.
The Pharmacopoeia of the People's Republic of China one of version in 2000 has been included kind Herba Clinopodii Tabellae.This medical instrument has effect of cooling blood and relieving pain.For dysfunctional uterine hemorrhage, postpartum hemorrhage, hematuria, hematemesis, has blood in stool, spitting of blood and traumatic hemorrhage etc.Use and show through preclinical phase, this medicine, for above-mentioned disease, has certain curative effect.
But the active component content of this medicine is lower, in the time of reply acute hemorrhage, effect is not remarkable, simultaneously because active component content is lower, causes this product dose larger, a 3-6 sheet, poor compliance while taking for the patient of old man, child and dysphagia.
Supercritical CO
2fluid extraction technology is the high-efficiency activated composition abstraction technique growing up this year, rises having a series of advantage aspect the extraction separation of Effective Component of Chinese Medicine compared with traditional method, as wide in opereating specification, be convenient to regulate, selectivity is good, and operative temperature is low, and it is destroyed etc. that active component is not easy.But, supercritical CO
2the disposable apparatus investment of fluid extraction technology is larger, give to popularize and bring certain difficulty, and supercritical extraction technique is not remarkable for the effect of extracting of some macromole polar substancess, makes its application in the field of Chinese medicines be subject to restriction to a certain degree.
To this, CN101301349A discloses a kind of by Duanxueliu extract oral freeze-dried tablet and preparation method thereof, adds appropriate amount of auxiliary materials to be mixed with solution, the oral freeze-dried slices of making through vacuum lyophilization taking Herba Clinopodii extract as active component.Duanxueliu extract oral freeze-dried tablet provided by the invention, mouthfeel is good, disintegrate fast (dissolving completely), taking convenience etc.
CN1939399A discloses a kind of blood flow cutting off dispersing tablet, taking Herba Clinopodii as raw material, prepares the fine powder of Herba Clinopodii extract, adds appropriate amount of auxiliary materials to make in 3 minutes disintegrate completely and reaches the blood flow cutting off dispersing tablet of homogeneously dispersed state, has cooling blood for hemostasis effect.
CN101543528A discloses a kind of clinopodium polycephalum aglycon oral formulations and its production and use, the total glycosides extracting from Herba Clinopodii is hydrolyzed, obtain clinopodium polycephalum aglycon, and coordinate special adjuvant to make high-efficiency preparation clinopodium polycephalum aglycon, can greatly improve the bioavailability of clinopodium polycephalum aglycon.Said preparation has obvious curative effect at treatment antiinflammatory and/or in treating the diseases such as wound, nose bleeding, gynecological bleeding.
But all there is following prominent question in above-mentioned these patents:
(1) adopt the active component in traditional method for extracting Herba Clinopodii, make the extraction ratio of active component low, active substance extracts not comprehensive, and impurity is more, and bioavailability is also not high enough;
(2) because its active constituent content is lower, the more extract that makes of impurity is anxious thick, and poor fluidity, is unfavorable for the follow-up film-making of product;
(3) content of drug effect components in product is low, needs to add more extract, and then make film-making difficulty in making perhaps to process, and tablet is not easy molding, to having relatively high expectations of follow-up transportation and packing;
(4) use the more complex process that makes of adjuvant, but to the curative effect of product almost without any beneficial effect.
To this, a kind of with good fluidity, content of drug effect components is high and bioavailability is high Herba Clinopodii extract be combined with the adjuvant of less kind prepare drug effect significantly, the Herba Clinopodii Tabellae that is easy to take is technical problem anxious to be resolved.
Summary of the invention
For addressing the above problem, the invention provides one for Herba Clinopodii Tabellae, specifically provide a kind of with supercritical CO
2the active component of fluid extraction technology extraction Herba Clinopodii is combined and is made tablet for cooling blood and relieving pain and preparation method thereof with adjuvant again.
A kind of Herba Clinopodii Tabellae, by Herba Clinopodii supercritical CO
2fluid extract and adjuvant composition, is characterized in that the Herba Clinopodii supercritical CO that contains 0.5-1% in described Herba Clinopodii Tabellae
2fluid extract, and in described Herba Clinopodii Tabellae, contain the Buddlejasaponins Ⅳb that is not less than by weight 0.32%.
A kind of Herba Clinopodii Tabellae, is characterized in that described microcrystalline cellulose excipients, cross-linking sodium carboxymethyl cellulose, pregelatinized Starch, processing agar, protein sugar, lactose.
A kind of Herba Clinopodii Tabellae, is characterized in that obtaining raw material by following weight proportioning makes: Herba Clinopodii supercritical CO
2fluid extract 0.5-1 part, microcrystalline Cellulose 25-35 part, cross-linking sodium carboxymethyl cellulose 30-45 part, pregelatinized Starch 8-12 part, processing agar 4-8 part, protein sugar 5-8 part, lactose 3-9 part.
A kind of Herba Clinopodii Tabellae, is characterized in that obtaining raw material by following weight proportioning makes: Herba Clinopodii supercritical CO
21 part of fluid extract, 32 parts of microcrystalline Cellulose, 38 parts of cross-linking sodium carboxymethyl celluloses, 10 parts of pregelatinized Starch, 6 parts of protein sugar, 7 parts of lactose.
A kind of Herba Clinopodii Tabellae, is characterized in that described Herba Clinopodii supercritical CO
2fluid extract is to be worth by the following method: get Herba Clinopodii, at 0-10 DEG C, grind, cross 10-30 mesh sieve; Herba Clinopodii powder after sieving adds supercritical CO
2in extraction equipment, extract extraction temperature 25-35 DEG C, extracting pressure 10-25MPa, CO
2flow 2-3L/h, the mode that adopts dynamic extraction to combine with dynamic extraction extracts, wherein first static extracting 10-15min, dynamic extraction 5-10min subsequently, it is an extraction cycle that a dynamic extraction adds a static extracting, repeat this circulation 1-3 time, when extraction, add in the dehydrated alcohol of Herba Clinopodii total amount 1.0-1.2ml/g and the N of 0.005-0.1g/g
2acyl amino acid type surfactant, carries out two-stage separation after having extracted, separation temperature is 20-30 DEG C, separating pressure 2-8MPa, isolated extracting solution recovery ethanol is obtained to extract for subsequent use.A kind of Herba Clinopodii Tabellae, is characterized in that described Herba Clinopodii supercritical CO
2fluid extract is to be worth by the following method: get Herba Clinopodii, at 10 DEG C, grind, cross 10 mesh sieves; Herba Clinopodii powder after sieving adds supercritical CO
2in extraction equipment, extract 25 DEG C of extraction temperature, extracting pressure 20MPa, CO
2flow 2L/h, the mode that adopts dynamic extraction to combine with dynamic extraction extracts, wherein first static extracting 10-15min, dynamic extraction 5-10min subsequently, it is an extraction cycle that a dynamic extraction adds a static extracting, repeat this circulation 2 times, when extraction, add in the dehydrated alcohol of Herba Clinopodii total amount 1.2ml/g and the N of 0.08g/g
2acyl amino acid type surfactant, carries out two-stage separation after having extracted, separation temperature is 25 DEG C, separating pressure 5MPa, isolated extracting solution recovery ethanol is obtained to extract for subsequent use.
A kind of Herba Clinopodii Tabellae, is characterized in that described Herba Clinopodii is carrying out supercritical CO
2before fluid extraction, the Herba Clinopodii powder after described sieving is carried out to microwave treatment, the power of described microwave treatment is 300-450W, and the processing time is 30-300s.
N2 acyl amino acid type surfactant of the present invention is preferably N
2acyl-lysine.
Herba Clinopodii Tabellae of the present invention has following beneficial effect
(1) first by supercritical CO
2fluid extraction technology is used for the extraction of Herba Clinopodii active ingredients of medicinal materials, and by a large amount of tests, its entrainer is screened, and finds to use N
2acyl-lysine can make extraction approach room temperature and lower atmospheric pressure carries out, and this makes to utilize supercritical CO
2the cost of fluid extraction technology reduces greatly, and in the product obtaining, the content of active component is higher, and thermal sensitivity composition is not destroyed;
(2) obtain a kind ofly without concentrated, in extract, just contain the Herba Clinopodii extract of at least 0.32% Buddlejasaponins Ⅳb.This extraction is directly carried out to film-making, the content of the contained effective ingredient of monolithic is increased greatly, and can dwindle the volume of tablet, the compliance while making this medicine for old man and child strengthens greatly, also makes this medicine be more suitable for emergency treatment.
(3) attempt first carrying out supercritical CO
2before fluid extraction, product is carried out to microwave treatment, prove microwave treatment and supercritical CO
2fluid extraction has significant synergism, can effectively improve the extraction ratio of its active component.
The detailed description of the invention of form by the following examples, is described in further detail foregoing of the present invention again.But this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following example, all technology realizing based on foregoing of the present invention all belong to scope of the present invention.
Detailed description of the invention
Embodiment 1
The preparation of Herba Clinopodii extract: get Herba Clinopodii, grind at 0-10 DEG C, cross 10 mesh sieves; Herba Clinopodii powder after sieving adds supercritical CO
2in extraction equipment, extract 25 DEG C of extraction temperature, extracting pressure 10MPa, CO
2flow 3L/h, the mode that adopts dynamic extraction to combine with dynamic extraction extracts, wherein first static extracting 15min, dynamic extraction 5min subsequently, it is an extraction cycle that a dynamic extraction adds a static extracting, repeat this circulation 1 time, when extraction, add in the dehydrated alcohol of Herba Clinopodii total amount 1.0ml/g and the N of 0.005g/g
2acyl amino acid type surfactant, carries out two-stage separation after having extracted, separation temperature is 25 DEG C, separating pressure 5MPa, isolated extracting solution recovery ethanol is obtained to extract for subsequent use.
Flaking method: get 32 parts of microcrystalline Cellulose, 38 parts of cross-linking sodium carboxymethyl celluloses, 10 parts of pregelatinized Starch, 6 parts of protein sugar, 7 parts of lactose, pulverized 60 mesh sieves; Add Herba Clinopodii supercritical CO
21 part of fluid extract and 90% alcoholic solution are appropriate, make soft material, and 40 mesh sieves are granulated, and 40 DEG C dry, control moisture 2.0%, with 20 mesh sieve granulate; Add and process 6 parts of mix homogeneously of agar, measuring point granule content, tabletting, regulate loading and pressure, hardness, sheet until tablet weigh after standard-required, carry out tabletting, within every 20 minutes, check once sheet weight, find that there is that loose sheet, sliver, sticking, tablet weight variation are excessive, variable color abnormal conditions are answered parking checking; Compacting plain sheet in blocks is added in high-efficiency coating machine, carry out film coating or sugar-coat, the sheet that dries in the air, outer package, to obtain final product.
Embodiment 2
Get Herba Clinopodii, at 10 DEG C, grind, cross 10 mesh sieves; Herba Clinopodii powder after sieving adds supercritical CO
2in extraction equipment, extract 25 DEG C of extraction temperature, extracting pressure 20MPa, CO
2flow 2L/h, the mode that adopts dynamic extraction to combine with dynamic extraction extracts, wherein first static extracting 10-15min, dynamic extraction 5-10min subsequently, it is an extraction cycle that a dynamic extraction adds a static extracting, repeat this circulation 2 times, when extraction, add in the dehydrated alcohol of Herba Clinopodii total amount 1.2ml/g and the N of 0.08g/g
2acyl-lysine, carries out two-stage separation after having extracted, separation temperature is 25 DEG C, separating pressure 5MPa, isolated extracting solution recovery ethanol is obtained to extract for subsequent use.Adopt the method film-making of embodiment 1.
Embodiment 3
Get Herba Clinopodii, at 10 DEG C, grind, cross 10 mesh sieves; Herba Clinopodii powder after sieving, in the microwave environment that is 400W as for power, is processed 60s, puts into subsequently supercritical CO
2in extraction equipment, extract 25 DEG C of extraction temperature, extracting pressure 20MPa, CO
2flow 2L/h, the mode that adopts dynamic extraction to combine with dynamic extraction extracts, wherein first static extracting 10-15min, dynamic extraction 5-10min subsequently, it is an extraction cycle that a dynamic extraction adds a static extracting, repeat this circulation 2 times, when extraction, add in the dehydrated alcohol of Herba Clinopodii total amount 1.2ml/g and the N of 0.08g/g
2acyl-lysine is entrainer, carries out two-stage separation after having extracted, and separation temperature is 25 DEG C, separating pressure 5MPa, isolated extracting solution recovery ethanol is obtained to extract for subsequent use.Adopt the method film-making of embodiment 1.
Control Example 1
The Herba Clinopodii Tabellae of preparing according to the method in Chinese Pharmacopoeia version in 2000.
Control Example 2
The blood flow cutting off dispersing tablet making according to the method for embodiment in CN1714808A 1.
Control Example 3
Get Herba Clinopodii, at 10 DEG C, grind, cross 10 mesh sieves; Herba Clinopodii powder after sieving adds supercritical CO
2in extraction equipment, extract 25 DEG C of extraction temperature, extracting pressure 20MPa, CO
2flow 2L/h, the mode that adopts dynamic extraction to combine with dynamic extraction extracts, wherein first static extracting 10-15min, dynamic extraction 5-10min subsequently, it is an extraction cycle that a dynamic extraction adds a static extracting, repeats this circulation 2 times, carries out two-stage separation after having extracted, separation temperature is 25 DEG C, separating pressure 5MPa, isolated extracting solution recovery ethanol is obtained to extract for subsequent use.Adopt the method film-making of embodiment 1.
Control Example 4
Get Herba Clinopodii, at 10 DEG C, grind, cross 10 mesh sieves; Herba Clinopodii powder after sieving adds supercritical CO
2in extraction equipment, extract 25 DEG C of extraction temperature, extracting pressure 20MPa, CO
2flow 2L/h, the mode that adopts dynamic extraction to combine with dynamic extraction extracts, wherein first static extracting 10-15min, dynamic extraction 5-10min subsequently, it is an extraction cycle that a dynamic extraction adds a static extracting, repeats this circulation 2 times, when extraction, add the dehydrated alcohol in Herba Clinopodii total amount 1.2ml/g, after having extracted, carry out two-stage separation, separation temperature is 25 DEG C, separating pressure 5MPa, isolated extracting solution recovery ethanol is obtained to extract for subsequent use.Adopt the method film-making of embodiment 1.
Prove beneficial effect of the present invention by the Buddlejasaponins Ⅳb content in Herba Clinopodii Tabellae and pharmacodynamics test below.
1. the mensuration of Buddlejasaponins Ⅳb in Herba Clinopodii Tabellae
Make Buddlejasaponins Ⅳb standard curve according to standard, preparative hplc condition: LichrospherC18 post (4.6mm × 250mm, 5 μ are m), measure wavelength: 250nm, mobile phase: methanol-water (80:20), flow velocity: 1mL/min, column temperature: 25 DEG C, sample size: 10 μ L.
Precision takes the Buddlejasaponins Ⅳb 5.08mg that is dried to constant weight in phosphorus pentoxide, dissolve with methanol standardize solution are in 25mL measuring bottle, therefrom pipette respectively 0.1, 0.5, 1.0, 2.0, 4.0, in 8.0mL to 10mL measuring bottle, methanol constant volume is to scale, be mixed with respectively 2.03, 10.16, 20.33, 40.66, 81.31, 162.62 the standard solution of μ g/mL, sample introduction 10 μ L respectively, measure in wavelength 250nm place, obtain equation of linear regression Y=11778X+97.169, R2=0.9998, Buddlejasaponins Ⅳb is linear within the scope of 2.03～162.62 μ g/mL.Application of sample recovery test, replica test, precision test, stability test all meet the requirements.
Buddlejasaponins Ⅳb content=(Buddlejasaponins Ⅳb quality/tablet quality) × 100%, measurement result is in table 1.
The content of Buddlejasaponins Ⅳb in the various Herba Clinopodii Tabellaes of table 1
| Sample number into spectrum | Buddlejasaponins Ⅳb content % |
| Embodiment 2 samples | 0.46*** |
| Embodiment 3 samples | 0.68*** |
| Control Example 1 sample | 0.17 |
| Control Example 2 samples | 0.55* |
| Control Example 3 samples | 0.096 |
| Control Example 4 samples | 0.23 |
(note: with the relatively * P < 0.005 of Herba Clinopodii Tabellae Isodose group of control Example 1; * P < 0.001, * * * P < 0.0001)
Can find out, Buddlejasaponins Ⅳb content % in embodiments of the invention 2 and embodiment 3 is far away higher than common Herba Clinopodii Tabellae, although there is not significant difference with the Buddlejasaponins Ⅳb content in control Example 2 samples in embodiment 2, but, it should be noted that, in embodiment 2, the content of Herba Clinopodii extract is only 1%, and the content of Herba Clinopodii extract is 23.58% in control Example 2, be not difficult to find out like this, the content of the active ingredient of the Herba Clinopodii Tabellae extract that extracting method of the present invention obtains is far away higher than control Example 2.
The Buddlejasaponins Ⅳb content of comparing embodiment 2, control Example 3 and control Example 4 can be found out, in the time adopting same condition to carry out supercritical extraction, if do not add entrainer, its active ingredient that can extract is very limited, although and only use the extraction quantity of its Buddlejasaponins Ⅳb of raising that ethanol can be by a relatively large margin as entrainer, but effect is still not remarkable, Buddlejasaponins Ⅳb extraction quantity basic and that decocting boils can not form significant difference, but uses the N that can produce acid and basic character
2when acyl-lysine, can find, Buddlejasaponins Ⅳb extraction quantity promotes greatly, has extremely significant difference (P < 0.0001) compared with the Buddlejasaponins Ⅳb extraction quantity of water decoction method.
Comparing embodiment 2 and embodiment 3 also can find out simultaneously, use microwave treatment Herba Clinopodii medical material powder can significantly improve the extraction quantity of Buddlejasaponins Ⅳb, prove to have synergism between microwave pretreatment and supercritical extraction.
2. the pharmacodynamics test of medicine dispersible tablet of the present invention
1, trial drug
The Herba Clinopodii Tabellae making according to the method for embodiment 2, embodiment 3, control Example 1 and control Example 2, specification: 0.3g/ sheet.Get 1 of Herba Clinopodii Tabellae, porphyrize, adds 3ml distilled water that compounding medicine is become to solution for standby.
2, statistical method
Use X2 method of inspection.
3, the effect of Herba Clinopodii Tabellae to isolated rabbit tremulous pulse bar
Get 1 of Japan large ear rabbit, the head of fiercelying attack is lethal at every turn.Open thoracic cavity and expose heart, separate aortic article.As far as possible near heart place clip aortic article, be placed in 5 DEG C of following krebs solutions of logical oxygen, one section of clip, carefully reject circumvascular tissue, carefully by vascular cuffing on the fine glass rod (diameter 3-4mm) of diameter and the same thickness of tremulous pulse, be cut into and be about 3-4cm with eye scissors, the spiral type silver of wide 3-4mm left and right.Two ends are threading ligation respectively, one end is fixed on glass ventilation hook, vertically be suspended from the maxwell bath pipe that fills 20ml krebs solution and (bathe pipe 37.5 ± 0.5 DEG C of the maintenances that are connected with thermostatic water-circulator bath, pH7.2-7.4, not open close with oxygen), the other end lies on the tonotransducer that is associated with monitor, load 2g tension force, and stablize 1.5-2 hour in bath pipe, then add 0.01% norepinephrine 0.1ml, inspection vasoconstrictor activity, when its effect peaks, rinse 3 times with krebs solution immediately, treat that it returns to the front level of administration, and after stable, add blood flow cutting off dispersing tablet 0.2ml, record shrinkage curve.Effect reaches behind peak, continues to record a period of time, and observation effect is held time.Then strengthen ventilation with krebs solution and rinse, treat that it returns to baseline, and stablize after 15 minutes, again add Herba Clinopodii Tabellae (ordinary tablet) 0.27g crude drug/ml medicinal liquid 0.2ml, recording curve, observes its effect peak and holds time.The changing value of contractility calculates in grams, can reflect from curve, converts and get final product.Experimental result is in table 2.
The effect of table 2 Herba Clinopodii Tabellae to rabbit aorta strip
Note: the Herba Clinopodii Tabellae Isodose group of * * and control Example 1 is P < 0.01 relatively
As can be seen from the table, Herba Clinopodii Tabellae of the present invention is to promote the time of peaking, tension force peak value all to have utmost point significant difference with acting duration compared with traditional Herba Clinopodii Tabellae, and also has significant difference compared with the blood flow cutting off dispersing tablet of control Example 2.Also it is to be noted, if do not use entrainer (control Example 3), be difficult to extract effective ingredient, thereby make its drug effect effect the poorest, use methanol as entrainer, although can extract a small amount of composition, but because its extraction temperature and pressure is all higher, same drug effect effect is bad.Can find out, Herba Clinopodii Tabellae of the present invention has significant curative effect at Zhixue Recipe mask.
Claims (8)
1. a Herba Clinopodii Tabellae, by Herba Clinopodii supercritical CO
2fluid extract and adjuvant composition, is characterized in that the Herba Clinopodii supercritical CO that contains 0.5-1% in described Herba Clinopodii Tabellae
2fluid extract, and in described Herba Clinopodii Tabellae, contain the Buddlejasaponins Ⅳb that is not less than by weight 0.32%.
2. a Herba Clinopodii Tabellae as claimed in claim 1, is characterized in that described microcrystalline cellulose excipients, cross-linking sodium carboxymethyl cellulose, pregelatinized Starch, protein sugar, lactose.
3. a Herba Clinopodii Tabellae as claimed in claim 2, is characterized in that obtaining raw material by following weight proportioning makes: Herba Clinopodii supercritical CO
2fluid extract 0.5-1 part, microcrystalline Cellulose 25-35 part, cross-linking sodium carboxymethyl cellulose 30-45 part, pregelatinized Starch 8-12 part, processing agar 4-8 part, protein sugar 5-8 part, lactose 3-9 part.
4. a Herba Clinopodii Tabellae as claimed in claim 4, is characterized in that obtaining raw material by following weight proportioning makes: Herba Clinopodii supercritical CO
21 part of fluid extract, 32 parts of microcrystalline Cellulose, 38 parts of cross-linking sodium carboxymethyl celluloses, 10 parts of pregelatinized Starch, 6 parts, agar of processing, 6 parts of protein sugar, 7 parts of lactose.
5. a Herba Clinopodii Tabellae as claimed in claim 1, is characterized in that described Herba Clinopodii supercritical CO
2fluid extract is to be worth by the following method: get Herba Clinopodii, at 0-10 DEG C, grind, cross 10-30 mesh sieve; Herba Clinopodii powder after sieving adds supercritical CO
2in extraction equipment, extract extraction temperature 25-35 DEG C, extracting pressure 10-25MPa, CO
2flow 2-3L/h, the mode that adopts dynamic extraction to combine with dynamic extraction extracts, wherein first static extracting 10-15min, dynamic extraction 5-10min subsequently, it is an extraction cycle that a dynamic extraction adds a static extracting, repeat this circulation 1-3 time, when extraction, add in the dehydrated alcohol of Herba Clinopodii total amount 1.0-1.2ml/g and the N of 0.005-0.1g/g
2acyl amino acid type surfactant, carries out two-stage separation after having extracted, separation temperature is 20-30 DEG C, separating pressure 2-8MPa, isolated extracting solution recovery ethanol is obtained to extract for subsequent use.
6. a Herba Clinopodii Tabellae as claimed in claim 5, is characterized in that described Herba Clinopodii supercritical CO
2fluid extract is to be worth by the following method: get Herba Clinopodii, at 10 DEG C, grind, cross 10 mesh sieves; Herba Clinopodii powder after sieving adds supercritical CO
2in extraction equipment, extract 25 DEG C of extraction temperature, extracting pressure 20MPa, CO
2flow 2L/h, the mode that adopts dynamic extraction to combine with dynamic extraction extracts, wherein first static extracting 10-15min, dynamic extraction 5-10min subsequently, it is an extraction cycle that a dynamic extraction adds a static extracting, repeat this circulation 2 times, when extraction, add in the dehydrated alcohol of Herba Clinopodii total amount 1.2ml/g and the N of 0.08g/g
2acyl amino acid type surfactant, carries out two-stage separation after having extracted, separation temperature is 25 DEG C, separating pressure 5MPa, isolated extracting solution recovery ethanol is obtained to extract for subsequent use.
7. a Herba Clinopodii Tabellae as claimed in claim 5, is characterized in that described Herba Clinopodii is carrying out supercritical CO
2before fluid extraction, the Herba Clinopodii powder after described sieving is carried out to microwave treatment, the power of described microwave treatment is 300-450W, and the processing time is 30-300s.
8. a Herba Clinopodii Tabellae of stating as claim 5, described N2 acyl amino acid type surfactant is preferably N
2acyl-lysine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410247510.9A CN103977071A (en) | 2014-06-06 | 2014-06-06 | Clinopodium polycephalum tablet and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410247510.9A CN103977071A (en) | 2014-06-06 | 2014-06-06 | Clinopodium polycephalum tablet and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103977071A true CN103977071A (en) | 2014-08-13 |
Family
ID=51269398
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410247510.9A Pending CN103977071A (en) | 2014-06-06 | 2014-06-06 | Clinopodium polycephalum tablet and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103977071A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116059226A (en) * | 2022-07-08 | 2023-05-05 | 安徽农业大学 | Application of buddleja saponin IVb in preparation of product for preventing and treating porcine epidemic diarrhea |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939399A (en) * | 2005-09-30 | 2007-04-04 | 江西本草天工科技有限责任公司 | Blood stream-breaking dispersing tablets |
-
2014
- 2014-06-06 CN CN201410247510.9A patent/CN103977071A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939399A (en) * | 2005-09-30 | 2007-04-04 | 江西本草天工科技有限责任公司 | Blood stream-breaking dispersing tablets |
Non-Patent Citations (3)
| Title |
|---|
| 徐先祥等: "超临界流体萃取在皂苷类成分提取中的应用", 《中国药房》 * |
| 王洋等: "夹带剂在超临界CO2萃取天然产物中的应用", 《食品研究与开发》 * |
| 罗登林等: "超声对超临界CO2反相微乳萃取人参皂甙的影响", 《江苏大学学报（自然科学版）》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116059226A (en) * | 2022-07-08 | 2023-05-05 | 安徽农业大学 | Application of buddleja saponin IVb in preparation of product for preventing and treating porcine epidemic diarrhea |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20160136224A1 (en) | Method for preparing a camellia nitidissima chi lipid-lowering and hypoglycemic agent | |
| CN101623394B (en) | Nakedflower beautyberry extract as well as preparation method, preparation and application thereof | |
| AU2014402938B2 (en) | Applications of phillyrin/phillygenin composition in preparing drugs or health care products for relieving and/or treating viral diseases | |
| RU2759382C2 (en) | Drug for injection based on saponin b4 pulsatilla | |
| WO2018058261A1 (en) | Traditional chinese medicine composition for treating psoriasis and preparation method thereof | |
| CN102228506A (en) | Composition of malaytea scurfpea extract as well as preparation method and use thereof | |
| WO2014014271A1 (en) | Tablet comprising melissa officinalis folium extract for preventing or treating angiogenesis or mmp activity-mediated disease | |
| JP2016539173A (en) | Oral solid preparations containing broad-kind grasses and total flavonoids, and uses thereof | |
| EP3572088B1 (en) | A panax plant extract and pharmaceutical composition and use thereof | |
| CN101890114A (en) | Li nation medicament extract and composition with bacteriostatic, anti-inflammatory and hemostasis effects and preparation method thereof | |
| WO2008145064A1 (en) | The method for a sequoyitol-containing extract obtaining from the genus of trifolium, sobyean and ginkgo biloba and use thereof | |
| CN102085344B (en) | Aplotaxis carminative sustained-release preparation and preparation method thereof | |
| CN103977071A (en) | Clinopodium polycephalum tablet and preparation method thereof | |
| CN102641342B (en) | A kind of Chinese medicine extract and preparation method for the treatment of nephropathy | |
| CN110403948A (en) | Phenylethanoid glycosides application in preparing anti-inflammatory drugs and preparation method thereof | |
| CN104435384B (en) | A kind of anti-inflammation slow releasing tablet | |
| CN103265493A (en) | Desmodium sequax extractive, as well as extraction method and new application thereof | |
| CN105796620A (en) | New applications of radix notoginseng and radix notoginseng extract to preparation of medicines for treating psoriasis | |
| CN101843669B (en) | Chinese medicinal effective-part composition for treating coronary heart diseases | |
| CN101019837B (en) | Ginnone ester dispersing table and its preparation method | |
| CN110302166A (en) | A kind of swap buffers tablet and preparation method thereof | |
| CN114848600B (en) | Fresh motherwort traditional Chinese medicine formula granule and preparation method thereof | |
| EP2340844A1 (en) | Anti-avian influenza virus agent, and product containing anti-avian influenza virus agent | |
| CN110448622B (en) | Medicine for treating heat type cold and preparation method and application thereof | |
| CN103251685B (en) | Rumex nepalensis spreng extract and application of the same in drug preparation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140813 |