CN1912614A - Method for controlling quality of andrographolide oral solid preparation - Google Patents
Method for controlling quality of andrographolide oral solid preparation Download PDFInfo
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- CN1912614A CN1912614A CN 200610115138 CN200610115138A CN1912614A CN 1912614 A CN1912614 A CN 1912614A CN 200610115138 CN200610115138 CN 200610115138 CN 200610115138 A CN200610115138 A CN 200610115138A CN 1912614 A CN1912614 A CN 1912614A
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- andrographolide
- oral solid
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- solid preparation
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Abstract
A method for controlling quality of andrographolide oral solid preparation applies high efficiency of liquid phase chromatography to detect content of andrographolide and work out digestion inspecting manner of andrographolide for controlling product quality effectively.
Description
Technical field
The present invention relates to method for controlling quality of andrographolide oral solid preparation, it is characterized in that adopting high performance liquid chromatography to detect andrographolide content, formulate andrographolide dissolution test method.
Background technology
The andrographolide assay adopts colourimetry and ultraviolet spectrophotometry respectively in the andrographolide bulk drug standard that one one of in 1977 version of Chinese Pharmacopoeia and national drug standards WS-10001-(HD-0971)-2002 record.The andrographolide sheet that one one of Chinese Pharmacopoeia in 1977, national drug standards WS3-B-3634-98 and WS-11086 (ZD-1086)-2002 record respectively, capsule standard be row dissolution test project not all, its assay also adopts colourimetry and ultraviolet spectrophotometry respectively, does not see the report that adopts high effective liquid chromatography for measuring andrographolide content.
Andrographolide is almost insoluble in water, and its oral solid formulation is difficult to guarantee that its clinical efficacy can get gives full play under the situation of no dissolution rate quality control standard.And adopting spectrophotometric method as the content detection means, relatively there are certain defective in its specificity, accuracy and accuracy etc. with high performance liquid chromatography.This shows that the andrographolide oral solid formulation still lacks the effective quality control method at present.
Goal of the invention
Defective at the existing quality standard existence of andrographolide oral solid formulation, the present invention adopts high performance liquid chromatography to detect andrographolide content, formulates andrographolide dissolution test method, reaches effective control product quality, guarantees the purpose of clinical efficacy.
Summary of the invention
For achieving the above object, the present invention by the following technical solutions:
1. content assaying method: according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica; With methyl alcohol one water (50: 50) is moving phase; The detection wavelength is 226nm.Number of theoretical plate calculates by the andrographolide peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing the andrographolide reference substance 25mg that is dried to constant weight through 105 ℃, put in the 50ml measuring bottle, it is an amount of to add methyl alcohol, behind the ultrasonic dissolution, add methyl alcohol to scale, shake up, filter, precision is measured subsequent filtrate 5ml, put in the 50ml measuring bottle, add moving phase and be diluted to scale, shake up, promptly.
The preparation sample thief of need testing solution, the accurate title, decide, porphyrize, precision takes by weighing in right amount (being equivalent to andrographolide 25mg approximately), puts in the 50ml measuring bottle, prepares with method.
Accurate respectively reference substance solution and each the 20 μ l injection liquid chromatograph of need testing solution drawn of determination method measured, promptly.
2. dissolution test method: sample thief, according to dissolution method (two appendix XC of Chinese Pharmacopoeia version pharmacopeia in 2005) second method, be dissolution medium with 10% ethanolic solution 1000ml respectively, rotating speed is that per minute 100 changes, operation in accordance with the law, in the time of 60 minutes, to get solution and filter, subsequent filtrate is as need testing solution; Precision takes by weighing andrographolide reference substance 10mg and puts in the 100ml measuring bottle, adds ethanol 10ml ultrasonic dissolution, and is diluted with water to scale, shakes up; Precision is measured 5ml and is put in the 100ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, in contrast product solution.Get reference substance solution and need testing solution respectively, measure absorbance log at wavelength 226nm place, calculate stripping quantity according to spectrophotometric method (appendix V of Chinese Pharmacopoeia version in 2005).
Beneficial effect of the present invention:
1. assay
1. linear relationship: andrographolide is the good linear relation with chromatographic peak area in 9.6～86 μ g/ml concentration ranges, correlation coefficient r is 0.9999.
2. measure the stability of solution: it is stable in 8 hours to measure solution.
3. limit of identification: by dilution method progressively, when signal to noise ratio (S/N ratio) was 3: 1, concentration limit was 0.29 μ g/ml.
4. precision: withinday precision RSD is 0.1%, and day to day precision RSD is 0.3%.
5. specificity: auxiliary material is noiseless to detecting.
6. the recovery: average recovery rate is 99.9%, and RSD is 0.18%.It is 98.3% that ultraviolet spectrophotometry detects average recovery rate, and RSD is 0.53%.
2. dissolution test
1. linear relationship: andrographolide is the good linear relation with absorbance log in 2.1 μ g～12.6 μ g/ml concentration ranges, correlation coefficient r is 0.9999.
2. measure the stability of solution: it is stable in 8 hours to measure solution.
3. specificity: auxiliary material is noiseless to detecting.
4. the recovery: average recovery rate is 100.1%, and RSD is 0.26%.
5. the selection of dissolution medium, stirring means, rotating speed: with 10% ethanolic solution 1000ml is that dissolution medium, stirring means are that slurry method, rotating speed are that per minute 100 commentaries on classics help andrographolide stripping inspection.
Claims (3)
1. method for controlling quality of andrographolide oral solid preparation is characterized in that adopting high performance liquid chromatography to detect andrographolide content, formulates andrographolide dissolution test method.
2. the described andrographolide oral solid formulation of claim 1 content assaying method is characterized in that with octadecylsilane chemically bonded silica be filling agent; With the methanol-water is moving phase; The detection wavelength is 226nm; The reference substance method is calculated andrographolide content.
3. the described andrographolide oral solid formulation of claim 1 dissolution test method, it is characterized in that according to two appendix XC of Chinese Pharmacopoeia version pharmacopeia in 2005 dissolution method, second method, be dissolution medium with 10% ethanolic solution 1000ml respectively, rotating speed is that per minute 100 changes, spectrophotometric method according to an appendix V regulation of Chinese Pharmacopoeia version in 2005, measure the absorbance log of solution at 226nm wavelength place, the reference substance method is calculated the andrographolide stripping quantity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610115138 CN1912614A (en) | 2006-08-26 | 2006-08-26 | Method for controlling quality of andrographolide oral solid preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610115138 CN1912614A (en) | 2006-08-26 | 2006-08-26 | Method for controlling quality of andrographolide oral solid preparation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1912614A true CN1912614A (en) | 2007-02-14 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610115138 Pending CN1912614A (en) | 2006-08-26 | 2006-08-26 | Method for controlling quality of andrographolide oral solid preparation |
Country Status (1)
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| CN (1) | CN1912614A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306082B (en) * | 2008-06-26 | 2011-03-09 | 广州奇星药业有限公司 | Houkangsan quality control method |
| CN103901147A (en) * | 2012-12-28 | 2014-07-02 | 天士力制药集团股份有限公司 | Method for measuring dissolution rate of andrographolide pills |
-
2006
- 2006-08-26 CN CN 200610115138 patent/CN1912614A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306082B (en) * | 2008-06-26 | 2011-03-09 | 广州奇星药业有限公司 | Houkangsan quality control method |
| CN103901147A (en) * | 2012-12-28 | 2014-07-02 | 天士力制药集团股份有限公司 | Method for measuring dissolution rate of andrographolide pills |
| CN103901147B (en) * | 2012-12-28 | 2018-04-03 | 天士力医药集团股份有限公司 | A kind of assay method of dripping pills of andrographolide dissolution rate |
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