CN102389445A - Angelica dahurica root dispensing granule and quality control thereof - Google Patents
Angelica dahurica root dispensing granule and quality control thereof Download PDFInfo
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- CN102389445A CN102389445A CN2011103734484A CN201110373448A CN102389445A CN 102389445 A CN102389445 A CN 102389445A CN 2011103734484 A CN2011103734484 A CN 2011103734484A CN 201110373448 A CN201110373448 A CN 201110373448A CN 102389445 A CN102389445 A CN 102389445A
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- angelicae dahuricae
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Abstract
Belonging to the field of traditional Chinese medicine extraction and preparations, the invention specifically relates to determination of a Chinese medicinal material, i.e. angelica dahurica roots, an angelica dahurica root dispensing granule, as well as its preparation method and quality control, and aims to provide an angelica dahurica root dispensing granule characterized by substantial product curative effect, stable quality and convenient administration. The product of the invention takes angelica anomala decoction pieces as the raw medicinal materials, which derive from the dry roots of Angelica dahurica (Fisch. Ex Hoffm.) Benth. et Hook. f. var. formosana (Boiss) Shan et Yuan and come from an angelica anomala GAP (good agricultural practice) base in Suining. The preparation method of the angelica dahurica root dispensing granule comprises the steps of: crushing the angelica anomala decoction pieces into coarse powder, immersing the powder with 50% ethanol for 24h, and conducting percolation at a dripping speed of 0.50ml/min; collecting six times the amount of the percolating liquid which is then subjected to concentration and spray drying, thus obtaining extract powder; adding an accessory about 15-50 wt% of the extract powder, then performing dry granulating, thus obtaining the granule. Quality identification and control of the angelica anomala decoction pieces and angelica dahurica root dispensing granule are both done through an HPLC (high performance liquid chromatography) fingerprint. The angelica dahurica root dispensing granule has the advantages of clear raw medicinal material source, controllable quality; simple production process and stable quality; substantial curative effect and convenient administration.
Description
Technical field
The invention belongs to Chinese medicine extraction and formulation art, be specifically related to the selection of Radix Angelicae Dahuricae Chinese crude drug, granule Radix Angelicae Dahuricae granule and preparation method thereof and method of quality control.
Background technology
The Radix Angelicae Dahuricae is for being the samphire Radix Angelicae Dahuricae
Angelica dahurica(Fisch. ex Hoffm.) Benth. et Hook. f or Radix angelicae dahuricae
Angelica dahurica(Fisch. ex Hoffm.) Benth. et Hook. f. var.
Formosana(Boiss.) dry root of Shan et Yuan.It is warm in nature, gas fragrance, and acrid in the mouth, little hardship are returned stomach, colon, lung meridian, have effects such as diffusing wind dehumidifying, sensible analgesia, detumescence and apocenosis.The Radix Angelicae Dahuricae is used as medicine and begins to be shown in " herbal classic ", classifies middle article as.Clinical treatment headache due to common cold, supraorbital bone pain, nasal obstruction, nasal sinusitis, toothache, leucorrhea and the skin infection card such as swell and ache that is mainly used in.For the ease of clinical practice, the Chinese medicine industry will meet the Chinese medicine decoction pieces of concocted specification as raw material, through modern crafts extract, concentrate, separate, dry, granulate, the refining granule that forms of packing.
Yet; Because the angelica root plant origin is different, results, processing and storing mode are different, and the influence of factor such as ecological environment; Can there be certain difference between the Radix Angelicae Dahuricae product in the different places of production; And unified quality standard standard control is not arranged at present as yet, cause the product quality disunity of different manufacturers, there is difference in drug effect; So be necessary Radix Angelicae Dahuricae granule is carried out quality control from each side such as crude drug, production technology, quality standard, pharmacological effects, a kind of determined curative effect, reliable quality Radix Angelicae Dahuricae granule be provided.
Summary of the invention
The objective of the invention is to disclose a kind of Radix Angelicae Dahuricae granule crude drug source; The present invention also aims to disclose the method for preparing of this formulation; The present invention also aims to disclose the method for quality control of this granule.
The objective of the invention is to realize through following technical scheme.
(1) Radix Angelicae Dahuricae granule crude drug confirms
The national commodity Radix Angelicae Dahuricae mainly contains " Qi Baizhi " (originating in Hebei), " Yu Baizhi " (originating in Henan), " Radix angelicae dahuricae " (originating in Zhejiang Hangzhou), " angelica anomala " (originating in Sichuan).This paper compares research to the Radix Angelicae Dahuricae of the different places of production, different processing methods, different commercial grade, different holding conditions: a. extractum, total coumarins, three kinds of coumarin component content contrasts; B. heavy metal, arsenic salt and persticide residue in each sample have been measured with the Chinese Pharmacopoeia method; C. the content of lead, hydrargyrum, cadmium, arsenic, copper in each sample of having used aas determination; D. want sulphuring because of Radix Angelicae Dahuricae processing at present more, still also to S, SO in the sample
2Content measure; E. to sulphuring and not the angelica root of sulphuring carried out the comparison of pharmacodynamics; The result shows: sulphuring Radix Angelicae Dahuricae sample does not demonstrate tangible analgesic effect; Can obviously reduce the mouse writhing number of times due to the glacial acetic acid, the sulphuring sample under same experimental condition does not then demonstrate analgesic effect.
According to above result of study, in conjunction with Radix Angelicae Dahuricae commodity market practical situation, confirm that the raw medicinal material of Radix Angelicae Dahuricae granule is an angelica anomala, derive from the samphire Radix angelicae dahuricae
Angelica dahurica(Fisch. ex Hoffm.) Benth. et Hook. f. var.
Formosana(Boiss) dry root of Shan et Yuan originates in angelica anomala GAP base, Suining.Excavate when leaf is yellow between summer, autumn, remove fibrous root and silt, dry or cold drying (can not sulphuring).
(2) method for preparing of Radix Angelicae Dahuricae granule is following:
Angelica anomala is ground into coarse powder, and 50% soak with ethanol 24h is with the fast percolation that drips of 0.50ml/min; Collect 6 times of amount percolates, the concentrated solution spray drying gets Radix Angelicae Dahuricae spray drying powder; The adjuvant that in Radix Angelicae Dahuricae spray drying powder, adds himself weight portion 15-50%, dry granulation, Radix Angelicae Dahuricae granule.
(3) quality control of angelica anomala medical material and Radix Angelicae Dahuricae granule
According to " quality standard of angelica anomala decoction pieces and Radix Angelicae Dahuricae granule is set up in 2010 editions requirements of Chinese pharmacopoeia respectively, comprises each item indexs such as character, the process of preparing Chinese medicine, discriminating, inspection, extractum, assay; Adopt HPLC to set up the finger printing of angelica anomala decoction pieces and Radix Angelicae Dahuricae granule, like accompanying drawing 1.
The specific embodiment
(1) process study
1. Study on extraction
Single factor has been investigated the influence of factors such as solvent concentration, percolation speed, medical material particle diameter, soak time, collecting amount to total coumarins content, imperatorin content and paste-forming rate.Through investigating, confirm that concentration of alcohol is 50%; The fast percolation that drips with 0.50ml/min; Angelica root breaks into coarse powder and extracts; Soak time is 24h; Collecting amount is 600ml.And having carried out confirmatory experiment with preferred process conditions, the result shows that this technology has repeatability, stablizes feasible.
2. impurity removal process research
By extraction process gained percolate paste-forming rate is 18% ~ 19%, according to " Chinese medicinal granule quality standard standardized study embodiment and requirement " unified suggestion, adopts two kinds of methods to examine or check centrifugal impurity-eliminating effect, and the result shows: centrifugal remove impurity is infeasible.Take directly to concentrate molding.
3. drying process research
According to " Chinese medicinal granule quality standard standardized study embodiment and requirement " unified suggestion, examination spray drying condition.
Medicinal liquid concentrates the back spray drying, is prone to sticking wall, makes adjuvant so add dextrin, and has examined or check supplementary product consumption.When the dextrin consumption be dried cream amount 50% the time, drying effect is better, can avoid sticking wall, obtains loose powder.
4. Study on Forming
According to " Chinese medicinal granule quality standard standardized study embodiment and requirement " unified suggestion, powder is with dry granulation after the employing spray drying.
(3) accomplished pilot scale research
According to the set technology of laboratory,, carried out pilot scale research by the requirement of granule.
Carry out pilot scale by set technology, enterprise possesses the corresponding apparatus condition, and medical material is beaten powder, percolation extraction, concentrating under reduced pressure, spray drying and dry granulation process and all carried out smoothly.Get the pilot scale finished product that every 1g is equivalent to crude drug 3g.Pilot scale research is the result show, the preparation technology of formulation rationally, stablize feasible.
(2) granule quality standard research
Use sample to carry out the research of quality standard through the preparation of the maturation process of pilot scale research.
1. the character of test agent during character is investigated 10 batches in conjunction with characteristic and method for makings such as the color of medical material, gas, flavors, has been confirmed the granule properties and characteristics.
2. differentiate and set up the TLC discrimination method; Carry out the HPLC finger printing research of granule by " Chinese medicine chromatographic fingerprinting experimentation technical manual (trying) " requirement, set up the HPLC fingerprint discrimination method of granule Coumarins composition.
3. inspection is by " relevant inspection has been carried out in the requirement of granule in appendix of Chinese pharmacopoeia version in 2010, all meets relevant regulations; By " correlation technique in 201 years version appendix of Chinese pharmacopoeia has carried out the limit examine of ash, acid-insoluble ash, heavy metal and arsenic salt, persticide residue; The content of the lead in the sample, hydrargyrum, cadmium, arsenic, copper that adopted aas determination.
4. the method for determination of extractives has been set up in determination of extractives, and the sample of different batches has been carried out assay.
5. assay has been set up the HPLC assay method of imperatorin content, the determined by ultraviolet spectrophotometry method of total coumarins constituents, and the centering test agent has carried out assay.
6. Radix Angelicae Dahuricae granule and our granule of preparation to domestic different manufacturers production carried out the comparative study of thin layer, coumarin composition and finger printing.
7. through having studied and defined the granule quality standard that controllability is high, specificity is strong.
(3) stability test research
Sample is under the condition of packing with aluminum-plastic composite membrane, and the preliminarily stabilised property in six months is good.Accelerated stability in three months is good, shows that the quality of Radix Angelicae Dahuricae granule is basicly stable.(0～32 ℃ of room temperature, relative humidity 50～80%, 0,1,2,3, June; 40 ℃ of temperature, relative humidity 75%, 0,1,2, March),
(4) research of the checking of main pharmacodynamics
According to the relevant regulations in " specification requirement of Chinese medicinal granule quality standard standardized study " (exposure draft); The pharmacodynamic index of selecting analgesia and this two Xiang Zuineng of antiinflammatory to represent Radix Angelicae Dahuricae function to cure mainly; Radix Angelicae Dahuricae granule and Radix Angelicae Dahuricae contrast decoction have been carried out pharmacodynamics comparative study; The result shows: Radix Angelicae Dahuricae granule demonstrates tangible analgesia and antiinflammatory action, and the contrast of the Radix Angelicae Dahuricae under same experimental condition decoction does not demonstrate analgesia and antiinflammatory action.It is thus clear that analgesia of Radix Angelicae Dahuricae granule and antiphlogistic drug effect obviously are superior to Radix Angelicae Dahuricae contrast decoction.
(5) safety evaluatio research
According to the relevant regulations in " specification requirement of Chinese medicinal granule quality standard standardized study " (exposure draft); The acute toxicity that has carried out the Radix Angelicae Dahuricae granule and Radix Angelicae Dahuricae contrast decoction compares; The result shows; Radix Angelicae Dahuricae granule (crude drug through ethanol extraction, concentrate, granulating forms) obvious than the acute toxicity of Radix Angelicae Dahuricae contrast decoction (crude drug boils through decocting), but still at scope (its LD of safe handling
50Be 348 times of clinical administration amount).So Radix Angelicae Dahuricae granule can be used safely clinically, also point out the toxic reaction that in use to note it simultaneously.
Claims (3)
1. Radix Angelicae Dahuricae granule, it is characterized in that: the raw medicinal material of Radix Angelicae Dahuricae granule is confirmed as angelica anomala, derives from the samphire Radix angelicae dahuricae
Angelica dahurica(Fisch. ex Hoffm.) Benth. et Hook. f. var.
Formosana(Boiss) dry root of Shan et Yuan originates in angelica anomala GAP base, Suining.
2. the method for preparing of a Radix Angelicae Dahuricae granule is characterized in that: adopt following method preparation:
Radix Angelicae Dahuricae decoction pieces is ground into coarse powder, and 50% soak with ethanol 24h is with the fast percolation that drips of 0.50ml/min; Collect 6 times of amount percolates, concentrate spray drying, extract powder; The adjuvant that adds himself weight portion 15-50% in the extract powder, dry granulation, Radix Angelicae Dahuricae granule.
3. the method for preparing of a Radix Angelicae Dahuricae granule, it is characterized in that: angelica anomala decoction pieces and Radix Angelicae Dahuricae granule all adopt the HPLC finger printing to carry out quality discrimination and control.
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| CN2011103734484A CN102389445A (en) | 2011-11-22 | 2011-11-22 | Angelica dahurica root dispensing granule and quality control thereof |
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| CN2011103734484A CN102389445A (en) | 2011-11-22 | 2011-11-22 | Angelica dahurica root dispensing granule and quality control thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108653348A (en) * | 2018-07-06 | 2018-10-16 | 亳州职业技术学院 | A kind of root of Dahurain angelica stem extraction Preparation Technology of Granules |
| CN109406681A (en) * | 2018-12-21 | 2019-03-01 | 广东方制药有限公司 | The UPLC characteristic spectrum construction method and detection method of angelica root |
| CN111289485A (en) * | 2020-03-13 | 2020-06-16 | 陕西中医药大学 | Simple method for identifying quality of angelica dahurica decoction pieces |
| CN113171297A (en) * | 2021-04-12 | 2021-07-27 | 湖北一正药业股份有限公司 | Production process of traditional Chinese medicine formula granules |
| CN115737569A (en) * | 2022-11-17 | 2023-03-07 | 天地恒一制药股份有限公司 | Preparation method of radix angelicae formula granules |
-
2011
- 2011-11-22 CN CN2011103734484A patent/CN102389445A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 高颖: "白芷配方颗粒质量标准的规范化研究", 《中国优秀硕士学位论文全文数据库 医药卫生科技辑》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108653348A (en) * | 2018-07-06 | 2018-10-16 | 亳州职业技术学院 | A kind of root of Dahurain angelica stem extraction Preparation Technology of Granules |
| CN109406681A (en) * | 2018-12-21 | 2019-03-01 | 广东方制药有限公司 | The UPLC characteristic spectrum construction method and detection method of angelica root |
| CN109406681B (en) * | 2018-12-21 | 2021-11-16 | 广东一方制药有限公司 | Construction method and detection method of UPLC characteristic spectrum of radix angelicae medicinal material |
| CN111289485A (en) * | 2020-03-13 | 2020-06-16 | 陕西中医药大学 | Simple method for identifying quality of angelica dahurica decoction pieces |
| CN113171297A (en) * | 2021-04-12 | 2021-07-27 | 湖北一正药业股份有限公司 | Production process of traditional Chinese medicine formula granules |
| CN115737569A (en) * | 2022-11-17 | 2023-03-07 | 天地恒一制药股份有限公司 | Preparation method of radix angelicae formula granules |
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Application publication date: 20120328 |