CN101810864A - Preparation method of volatile oil beta-cyclodextrin inclusion compound - Google Patents
Preparation method of volatile oil beta-cyclodextrin inclusion compound Download PDFInfo
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- CN101810864A CN101810864A CN201010152966A CN201010152966A CN101810864A CN 101810864 A CN101810864 A CN 101810864A CN 201010152966 A CN201010152966 A CN 201010152966A CN 201010152966 A CN201010152966 A CN 201010152966A CN 101810864 A CN101810864 A CN 101810864A
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Abstract
The invention discloses a preparation method of a volatile oil beta-cyclodextrin inclusion compound, which is characterized in that volatile oil is extracted from capillary artemisia, cabline patchouli, rhizoma atractylodis macrocephaiae, tangerine peel and rhizoma alismatis, and the inclusion compound is prepared through inclusion of beta-cyclodextrin. The volatile oil beta-cyclodextrin inclusion compound prepared in the method has a high inclusion rate.
Description
Technical field
The invention belongs to medical technical field, be specifically related to a kind of preparation method of volatile oil beta-cyclodextrin inclusion compound.
Background technology
Cyclodextrin (Cyclodextrin, be called for short CD) is the cyclic oligomer sugar compounds that is formed by connecting by α-1,4 glycosidic bond that starch obtains after the enzymolysis cyclization, is good enclose material.Its main component is that 6,7,8 glucose cyclizations are called α-CD, β-CD, γ-CD.Owing to produced the restriction of enzyme antibacterial and isolation technics etc., domestic industry production at present and application only be one kind of β-CD, cyclodextrin has the tubular structure of annular hollow, make it to form " ultra micro capsule " material with other compound molecule, thereby change the physicochemical property of object, in pharmaceutical preparation, brought into play positive role.Cyclodextrin not only has good enclose performance to chemicals, at field of medicaments extensive studies and application is arranged also.
At present, to use maximum in Chinese medicine preparation be to seal volatile ingredient to cyclodextrin.After volatile ingredient is sealed by cyclodextrin, can prevent its loss, improve stability of formulation.Have very strong volatility as paeonol, behind 40 ℃ of placement 10d, its residual rate only has 27%; And after making paeonol-β-CD, its residual rate is still more than 95% under the same conditions.Oleum Bulbus Allii-β-CD is 93% at 40 ℃ of residual rates of placing 3 months, and Oleum Bulbus Allii mixture its residual rate only surplus 6% with this understanding.Niaosaitong tablets has multiple volatile oil components such as Fructus Foeniculi, Pericarpium Citri Reticulatae, and former preparation technology directly sprays into tabletting behind the dried granule with volatile oil, and the tablet surface that makes often has oil mark, the time grow slightly black-film, quality of the pharmaceutical preparations instability.New technology is carried out β-CD with volatile oil and is sealed, and has overcome tablet oil impregnate phenomenon, has improved the quality of the pharmaceutical preparations greatly.The Rhizoma Cyperi ball is the preparation that Chinese Pharmacopoeia records, and its composition mostly is the former powder of the more Chinese medicine of oil content and forms.Because this pill dose is bigger, disintegrate is slow, and its volatile oil is bigger at preparation and storage process loss, influences its quality of the pharmaceutical preparations and use.Song Qingjun etc. extract the volatile oil in the Rhizoma Cyperi ball raw material, carry out enclose with β-CD, and then have made the Rhizoma Cyperi capsule, make disintegration of said preparation fast 0.5h, and reduce scattering and disappearing of volatile oil, improved curative effect.Seal volatile oil with cyclodextrin, also have guaiacol, Oleum Curcumae, cinnamic aldehyde and methyl cinnamate, ethyl ester, bufogenin, Pericarpium Citri Reticulatae volatile oil, Resina Ferulae oil, Rhizoma Zingiberis Recens volatile oil etc. with the example that improves preparation stability.
Summary of the invention
For these reasons, the scientific research personnel of the court is in fat proheparin new drug preparation research, Herba Artemisiae Scopariae, Herba Pogostemonis, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Rhizoma Alismatis are extracted the volatile oil that obtains and study, the process test of many times has been determined the inclusion method of β-CD, and this method has fine inclusion rate to the volatile oil of 5 kinds of Chinese medicines.
The present invention is achieved through the following technical solutions.
A kind of preparation method of volatile oil beta-cyclodextrin inclusion compound is got Herba Artemisiae Scopariae, Herba Pogostemonis, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Rhizoma Alismatis, adds water, and soaked overnight is extracted volatile oil with the way of distillation, collects Aromatic water, and the gained Aromatic water adds anhydrous Na with petroleum ether extraction
2SO
4Petroleum ether is reclaimed in dehydration, gets volatile oil, the weight of volatile oil volume and beta-schardinger dextrin-and water volume adopt saturated water solution method, in 30 ℃ of-50 ℃ of water-baths with the ratio of 0.5-1.5: 4-8: 15-25, stirred enclose 60-120 minute, and put and be chilled to room temperature, in 2-4 ℃ of placement, sucking filtration, is put in the baking oven to there not being fragranced with petroleum ether filter wash cake, dry, get volatile oil beta cyclodextrin inclusion complex, divide and get ether layer in the cleaning mixture, add anhydrous Na
2SO
4Petroleum ether is reclaimed in dehydration, obtains volatile oil, with the method enclose, merges the gained clathrate twice.
The weight of its preferred volatile oil volume and beta-schardinger dextrin-and water volume were with 1: 6: 20 ratio.
Fat proheparin volatile oil beta cyclodextrin inclusion complex Study on Preparation
Preliminary animal pharmacology evidence, volatile oil has certain pharmacologically active.Volatile oil is volatile lost, oxidation deterioration in extraction, storage process.In order to keep volatile oil component as much as possible, use beta-cyclodextrin inclusion compound volatile oil, can reduce that the volatilization of volatile oil in preparation production, storage process scattered and disappeared, oxidation deterioration, thereby improve stability of formulation.In order to adapt to production, with reference to relevant document, adopt simple to operate, the saturated water solution method that equipment requirements is not high, and with oil with beta-schardinger dextrin-proportioning, enclose temperature, mixing time be factor, respectively get three levels, be evaluation index with the inclusion rate (weight coefficient 0.8) of volatile oil and the recovery rate (weight coefficient 0.2) of clathrate, carry out L9 (34) orthogonal test, screen best inclusion condition.
(1) Orthogonal Experiment and Design
1. evaluation index
2. the factor level table sees Table 1
Table 1 fat proheparin volatile oil beta cyclodextrin inclusion complex preparation factor water-glass
(2) test method
1. L9 (34) orthogonal test calendar medium oil and beta-schardinger dextrin-proportioning are pressed in the clathrate preparation, and precision takes by weighing an amount of beta-schardinger dextrin-, makes saturated aqueous solution in water bath with thermostatic control, under electronic stirring, the alcoholic solution (50%V/V) of an amount of volatile oil is added drop-wise in the beta-schardinger dextrin-saturated solution, and constant temperature stirs certain hour, stops heating and stirring, put to room temperature, in 2-4 ℃ of cold preservation 24h, sucking filtration, filter cake is washed till no fragranced with petroleum ether (30-60 ℃ of boiling range), put in 40 ℃ of baking ovens drying.
2. volatile oil contents is measured according to " an appendix XD of Chinese pharmacopoeia version in 2000 determination of volatile oil Division A League Matches of French Football method is measured in the clathrate.
(3) test arrangement and result see Table 2,3
Table 2 fat proheparin volatile oil beta cyclodextrin inclusion complex prepares orthogonal experiment arrangement and result
Inclusion rate scoring=inclusion rate/maximum inclusion rate * 0.8 * 100
Recovery rate scoring=recovery rate/maximum recovery rate * 0.2 * 100
Table 3 fat proheparin volatile oil beta cyclodextrin inclusion complex prepares variance analysis
F
0.05(2，2)＝19.00
By table 2,3 as seen, influences the inclusion process factors and be followed successively by A＞B＞C, and promptly oil is remarkable to the clathrate process influence with the proportioning and the enclose temperature of beta-schardinger dextrin-, and the mixing time influence is very little, so best enclose condition is A
2B
2C
2, promptly with 6 times of beta-cyclodextrin inclusion compounds to the volatilization oil mass, the enclose temperature is 40 ℃, the enclose time is 90min..
(4) demonstration test is with optimum process condition A
2B
2C
2, the material of getting it filled carries out demonstration test, the results are shown in Table 3
Three crowdes of confirmatory experiment results of table 3
Checking is the result show, selected stable process conditions is reliable, can be used as the preparation technology of fat proheparin volatile oil beta cyclodextrin inclusion complex.
Annotate: the described fat proheparin of above-mentioned test volatile oil is the volatile oil of Herba Artemisiae Scopariae, Herba Pogostemonis, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Rhizoma Alismatis extraction.
Preparation embodiment
Embodiment 1
Get Herba Artemisiae Scopariae, Herba Pogostemonis, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Rhizoma Alismatis, add water, soaked overnight is extracted volatile oil with the way of distillation, collects Aromatic water, and the gained Aromatic water adds anhydrous Na with petroleum ether extraction
2SO
4Petroleum ether is reclaimed in dehydration, gets volatile oil, the weight of volatile oil volume and beta-schardinger dextrin-and water volume adopt saturated water solution method, in 30 ℃ of water-baths with 0.5: 4: 15 ratio, stirred enclose 120 minutes, and put and be chilled to room temperature, in 2-4 ℃ of placement, sucking filtration, is put in the baking oven to there not being fragranced with petroleum ether filter wash cake, dry, get volatile oil beta cyclodextrin inclusion complex, divide and get ether layer in the cleaning mixture, add anhydrous Na
2SO
4Petroleum ether is reclaimed in dehydration, obtains volatile oil, with the method enclose, merges the gained clathrate twice.
Embodiment 2
: get Herba Artemisiae Scopariae, Herba Pogostemonis, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Rhizoma Alismatis, add water, soaked overnight is extracted volatile oil with the way of distillation, collects Aromatic water, and the gained Aromatic water adds anhydrous Na with petroleum ether extraction
2SO
4Petroleum ether is reclaimed in dehydration, gets volatile oil, the weight of volatile oil volume and beta-schardinger dextrin-and water volume adopt saturated water solution method, in 50 ℃ of water-baths with 1.5: 8: 25 ratio, stirred enclose 60 minutes, and put and be chilled to room temperature, in 2-4 ℃ of placement, sucking filtration, is put in the baking oven to there not being fragranced with petroleum ether filter wash cake, dry, get volatile oil beta cyclodextrin inclusion complex, divide and get ether layer in the cleaning mixture, add anhydrous Na
2SO
4Petroleum ether is reclaimed in dehydration, obtains volatile oil, with the method enclose, merges the gained clathrate twice.
Embodiment 3
Get Herba Artemisiae Scopariae, Herba Pogostemonis, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Rhizoma Alismatis, add water, soaked overnight is extracted volatile oil with the way of distillation, collects Aromatic water, and the gained Aromatic water adds anhydrous Na with petroleum ether extraction
2SO
4Petroleum ether is reclaimed in dehydration, gets volatile oil, the weight of volatile oil volume and beta-schardinger dextrin-and water volume adopt saturated water solution method, in 35 ℃ of water-baths with 0.8: 5: 16 ratio, stirred enclose 110 minutes, and put and be chilled to room temperature, in 2-4 ℃ of placement, sucking filtration, is put in the baking oven to there not being fragranced with petroleum ether filter wash cake, dry, get volatile oil beta cyclodextrin inclusion complex, divide and get ether layer in the cleaning mixture, add anhydrous Na
2SO
4Petroleum ether is reclaimed in dehydration, obtains volatile oil, with the method enclose, merges the gained clathrate twice.
Embodiment 4
Get Herba Artemisiae Scopariae, Herba Pogostemonis, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Rhizoma Alismatis, add water, soaked overnight is extracted volatile oil with the way of distillation, collects Aromatic water, and the gained Aromatic water adds anhydrous Na with petroleum ether extraction
2SO
4Petroleum ether is reclaimed in dehydration, gets volatile oil, the weight of volatile oil volume and beta-schardinger dextrin-and water volume adopt saturated water solution method, in 45 ℃ of water-baths with 1.2: 7: 23 ratio, stirred enclose 75 minutes, and put and be chilled to room temperature, in 2-4 ℃ of placement, sucking filtration, is put in the baking oven to there not being fragranced with petroleum ether filter wash cake, dry, get volatile oil beta cyclodextrin inclusion complex, divide and get ether layer in the cleaning mixture, add anhydrous Na
2SO
4Petroleum ether is reclaimed in dehydration, obtains volatile oil, with the method enclose, merges the gained clathrate twice.
Embodiment 5
Get Herba Artemisiae Scopariae, Herba Pogostemonis, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Rhizoma Alismatis, add water, soaked overnight is extracted volatile oil with the way of distillation, collects Aromatic water, and the gained Aromatic water adds anhydrous Na with petroleum ether extraction
2SO
4Petroleum ether is reclaimed in dehydration, gets volatile oil, the weight of volatile oil volume and beta-schardinger dextrin-and water volume adopt saturated water solution method, in 40 ℃ of water-baths with 1: 6: 20 ratio, stirred enclose 90 minutes, and put and be chilled to room temperature, in 2-4 ℃ of placement, sucking filtration, is put in the baking oven to there not being fragranced with petroleum ether filter wash cake, dry, get volatile oil beta cyclodextrin inclusion complex, divide and get ether layer in the cleaning mixture, add anhydrous Na
2SO
4Petroleum ether is reclaimed in dehydration, obtains volatile oil, with the method enclose, merges the gained clathrate twice.
Claims (2)
1. the preparation method of a volatile oil beta-cyclodextrin inclusion compound, it is characterized in that: get Herba Artemisiae Scopariae, Herba Pogostemonis, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Rhizoma Alismatis, add water, soaked overnight is extracted volatile oil with the way of distillation, collects Aromatic water, and the gained Aromatic water adds anhydrous Na with petroleum ether extraction
2SO
4Petroleum ether is reclaimed in dehydration, gets volatile oil, the weight of volatile oil volume and beta-schardinger dextrin-and water volume adopt saturated water solution method, in 30 ℃ of-50 ℃ of water-baths with the ratio of 0.5-1.5: 4-8: 15-25, stirred enclose 60-120 minute, and put and be chilled to room temperature, in 2-4 ℃ of placement, sucking filtration, is put in the baking oven to there not being fragranced with petroleum ether filter wash cake, dry, get volatile oil beta cyclodextrin inclusion complex, divide and get ether layer in the cleaning mixture, add anhydrous Na
2SO
4Petroleum ether is reclaimed in dehydration, obtains volatile oil, with the method enclose, merges the gained clathrate twice.
2. preparation method according to claim 1, the weight of its volatile oil volume and beta-schardinger dextrin-and water volume were with 1: 6: 20 ratio.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102000236A (en) * | 2010-11-23 | 2011-04-06 | 康美药业股份有限公司 | Method for preparing volatile oil inclusion compound and application thereof |
| CN102188738A (en) * | 2010-12-21 | 2011-09-21 | 舒明宇 | Preparation method of cyclodextrin inclusion compound and application of cyclodextrin inclusion compound in decorations |
| CN102861299A (en) * | 2012-10-22 | 2013-01-09 | 成都中医药大学附属医院 | Drug composition for treating depressive disorders, preparation method and application of drug composition |
| CN106822919A (en) * | 2017-03-14 | 2017-06-13 | 胡江宇 | A kind of peppermint oil sustained release inclusion compound and preparation method thereof |
| CN107212408A (en) * | 2017-06-20 | 2017-09-29 | 苏州市李良济健康产业有限公司 | A kind of preparation method for the health products for improving memory |
| CN107474962A (en) * | 2017-06-30 | 2017-12-15 | 河北中医学院 | A kind of earlier stage treatment process containing volatile oil clathrate compound |
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2010
- 2010-04-22 CN CN201010152966A patent/CN101810864A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102000236A (en) * | 2010-11-23 | 2011-04-06 | 康美药业股份有限公司 | Method for preparing volatile oil inclusion compound and application thereof |
| CN102000236B (en) * | 2010-11-23 | 2012-05-23 | 康美药业股份有限公司 | Method for preparing volatile oil inclusion compound and application thereof |
| CN102188738A (en) * | 2010-12-21 | 2011-09-21 | 舒明宇 | Preparation method of cyclodextrin inclusion compound and application of cyclodextrin inclusion compound in decorations |
| CN102861299A (en) * | 2012-10-22 | 2013-01-09 | 成都中医药大学附属医院 | Drug composition for treating depressive disorders, preparation method and application of drug composition |
| CN106822919A (en) * | 2017-03-14 | 2017-06-13 | 胡江宇 | A kind of peppermint oil sustained release inclusion compound and preparation method thereof |
| CN107212408A (en) * | 2017-06-20 | 2017-09-29 | 苏州市李良济健康产业有限公司 | A kind of preparation method for the health products for improving memory |
| CN107474962A (en) * | 2017-06-30 | 2017-12-15 | 河北中医学院 | A kind of earlier stage treatment process containing volatile oil clathrate compound |
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Application publication date: 20100825 |