CN102836207A - Preparation process of hydrochloric acid stachydrine extract and quality control method thereof - Google Patents
Preparation process of hydrochloric acid stachydrine extract and quality control method thereof Download PDFInfo
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- CN102836207A CN102836207A CN2012103605312A CN201210360531A CN102836207A CN 102836207 A CN102836207 A CN 102836207A CN 2012103605312 A CN2012103605312 A CN 2012103605312A CN 201210360531 A CN201210360531 A CN 201210360531A CN 102836207 A CN102836207 A CN 102836207A
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Abstract
The invention discloses a preparation process of a hydrochloric acid stachydrine extract and a quality control method thereof. The preparation process for the extract comprises the steps as follows: adding 10 to 15 times of amount of water to 10kg of herba leonuri medicinal material; heating, refluxing and extracting for 2 to 5h; filtrating, concentrating the filtrate to 5,000ml; adding the equivalent of 70% of ethanol to extract for 1 to 3 times; filtrating and washing the filter residues with 50% of ethanol; mixing the eluent with the filtrate; decompressing, concentrating and recovering the ethanol to obtain an extract with the relative density of 1.10 to 1.30 at 60 DEG.C. According to the invention, the quality of the hydrochloric acid stachydrine extract is controlled by utilizing a high performance liquid chromatography. The preparation process provided by the invention has the advantages that the process parameters, the process conditions and the process technology are stable; the extraction yield of the hydrochloric acid stachydrine extract is high; and the industrial applicability is strong. The quality control method provided by the invention has the advantages of high degree of separation, good linear relation, convenience, rapidness, accuracy and stability. Therefore, the quality control method meets the requirements of the industrial production and effectively controls the quality of the hydrochloric acid stachydrine extract and a preparation thereof.
Description
Technical field
The present invention relates to a kind of stachydrine hydrochloride extract making method and product quality control method.
Background technology
Herba Leonuri is the dry stem and leaf of labiate Herba Leonuri Leonurus heterophyllus Sweet..Be distributed widely in all parts of the country, Herba Leonuri main chemical compositions and effective ingredient are alkaloids, mainly contain stachydrine, leonurine etc.Rapid-action, the persistent of oral formulations such as the tablet of processing with this stachydrine extractum, capsule, drop pill, granulation machine.
YIMUCAO PIAN national standard (WS
3-B-2603-97) put down in writing the preparation and the content assaying method of this stachydrine hydrochloride extractum; But this method for preparing technological parameter, process conditions and Technology are unreasonable; Extraction the rate of extract is low; Its content assaying method adopts Reinecke salt sedimentation method to measure Determination of Contents of Hydrochloric Stachydrine, and complex operation, poor stability, error are big.Therefore, existing preparation of YIMUCAO PIAN and content control method can not adapt to the commercial production demand in ground, and product quality is difficult to be effectively controlled.
Summary of the invention
For solving the deficiency of above-mentioned prior art, the invention provides a kind of preparation and method of quality control thereof of stachydrine hydrochloride extractum, short to realize preparation time, it is high to extract the rate of extract; And the employing HPLC is easy, measure Determination of Contents of Hydrochloric Stachydrine quickly and accurately.
The present invention solves the problems of the technologies described above with following technical scheme:
Stachydrine hydrochloride extract making method of the present invention, its operational approach is following:
Get Herba Leonuri medical material 10kg and add 10 ~ 15 times of water gagings, heating and refluxing extraction 2 ~ 5 hours filters; Filtrating is concentrated into 5000ml, adds equivalent 70% ethanol extraction 1 ~ 3 time, filters; Filtering residue is used 50% washing with alcohol; Washing liquid merges with filtrating, and relative density was 1.10 ~ 1.30 extractum when concentrating under reduced pressure reclaimed ethanol to 60 ℃, promptly got.
The method of quality control of stachydrine hydrochloride extractum of the present invention, its operational approach is following:
Chromatographic condition and system suitability: adopt amino chromatographic column, with Yi Jing ︰ water by volume=solution of 75:25 mixed preparing is mobile phase, the detection wavelength is 198nm.
The preparation of reference substance solution: it is an amount of to get the stachydrine hydrochloride reference substance, and precision steelyard is fixed, adds the solution that methanol is processed the hydrochloric stachydrine 100 μ g of 1ml, as reference substance solution.
Supply the preparation of examination device solution: get stachydrine hydrochloride extractum 0.1g, precision steelyard is fixed, puts in the 50ml measuring bottle, and it is an amount of to add ethanol, and supersound process (power 250W, frequency 33KHz), shakes up to the 50ml scale with ethanol dilution, filters, and gets this filtrating, as need testing solution.
Algoscopy: accurate respectively above-mentioned reference substance and each 20 μ l of need testing solution of drawing, inject high performance liquid chromatograph, according to high effective liquid chromatography for measuring, promptly get.
Extract making method of the present invention, preparation time is short, and it is high to extract the rate of extract, and ethanol is recyclable to be utilized again, reduces energy waste.
The stachydrine extractum that adopts the inventive method to process can be processed oral formulations such as tablet, capsule, drop pill, granulation machine.
The present invention controls the quality of stachydrine hydrochloride extractum with HPLC, and method is simple and efficient, accurately stable, can adapt to industrial needs, can control the quality of stachydrine hydrochloride extractum and preparation thereof effectively.
The specific embodiment
Embodiment 1 (preparation of stachydrine hydrochloride extractum)
Get the water that Herba Leonuri medical material 10kg adds 10 times of weight, be heated to 100 ℃, reflux, extract, 2 hours; Filter, filtrating is concentrated into 5000ml, adds equivalent volumes concentration and be 70% ethanol extraction 2 times; Filter, filtering residue use volumetric concentration is 50% washing with alcohol, and washing liquid merges with filtrating; It is the extractum of 1.10 (60 ℃) that concentrating under reduced pressure reclaims ethanol to relative density, promptly gets.
Embodiment 2 (preparation of stachydrine hydrochloride extractum)
Get the water that Herba Leonuri medical material 10kg adds 13 times of weight, be heated to 100 ℃, reflux, extract, 3 hours; Filter, filtrating is concentrated into 5000ml, adds equivalent volumes concentration and be 70% ethanol extraction 3 times; Filter, filtering residue use volumetric concentration is 50% washing with alcohol, and washing liquid merges with filtrating; It is the extractum of 1.20 (60 ℃) that concentrating under reduced pressure reclaims ethanol to relative density, promptly gets.
Embodiment 3 (preparation of stachydrine hydrochloride extractum)
Get the water that Herba Leonuri medical material 10kg adds 15 times of weight, be heated to 100 ℃, reflux, extract, 4 hours; Filter, filtrating is concentrated into 5000ml, adds equivalent volumes concentration and be 70% ethanol extraction 2 times; Filter, filtering residue use volumetric concentration is 50% washing with alcohol, and washing liquid merges with filtrating; It is the extractum of 1.30 (60 ℃) that concentrating under reduced pressure reclaims ethanol to relative density, promptly gets.
Embodiment 4 (method of quality control of stachydrine hydrochloride extractum)
Chromatographic condition and system suitability: adopt amino chromatographic column, with Yi Jing ︰ water by volume=solution of 75:25 mixed preparing is mobile phase, the detection wavelength is 198nm.
The preparation of reference substance solution: it is an amount of to get the stachydrine hydrochloride reference substance, and precision steelyard is fixed, adds the solution that absolute methanol is processed the hydrochloric stachydrine 100 μ g of 1ml, as reference substance solution.
Supply the preparation of examination device solution: get stachydrine hydrochloride extractum 0.1g, precision steelyard is fixed, puts in the 50ml measuring bottle; It is an amount of to add volumetric concentration 70% ethanol, supersound process (power 250W, frequency 33KHz);, shake up to the 50ml scale with volumetric concentration 70% ethanol dilution, filter; Get this filtrating, as need testing solution.
Algoscopy: accurate respectively above-mentioned reference substance and each 20 μ l of need testing solution of drawing, inject high performance liquid chromatograph, measure according to HPLC (2010 editions one appendix VI D of Chinese Pharmacopoeia), promptly get.
Industrial applicibility is investigated
1, adopt Determination of Contents of Hydrochloric Stachydrine in the high effective liquid chromatography for measuring stachydrine hydrochloride extractum according to the invention, its result shows that stachydrine hydrochloride chromatographic peak area in 6.8～54.4 μ g/ml scopes is good linear with solution concentration and concerns that r is 0.9999; Separating degree is good, and theoretical cam curve is calculated as 7506 by the stachydrine hydrochloride peak; When signal to noise ratio was 2:1, sample minimum detectable concentration was 0.15 μ g/ml; It is stable in 10 hours to measure solution; Stachydrine hydrochloride assay average recovery rate is 99.8%, and RSD is 0.32%; Precision test RSD is 0.73%; Stability test RSD is 0.95%.
2, the foregoing description all adopts with a collection of Herba Leonuri medical material; Detect above embodiment 1 ~ embodiment 3 prepared stachydrine hydrochloride extractum Determination of Contents of Hydrochloric Stachydrine with HPLC of the present invention and be respectively 5.12%, 6.62% and 5.03%, the stachydrine hydrochloride extract yield is respectively 78.8%, 82.5% and 75.2%.
In sum, stachydrine hydrochloride extract making method technological parameter of the present invention, process conditions and stable technology, extraction time is short, and yield is high, and industrial applicibility is strong; The present invention controls the quality of stachydrine hydrochloride extractum with HPLC, and method is simple and efficient, accurately stable, can adapt to industrial needs, can control the quality of stachydrine hydrochloride extractum and preparation thereof effectively.
Claims (2)
1. a stachydrine hydrochloride extract making method is characterized in that, its operational approach is following:
Get Herba Leonuri medical material 10kg and add 10 ~ 15 times of water gagings, heating and refluxing extraction 2 ~ 5 hours filters; Filtrating is concentrated into 5000ml, adds equivalent 70% ethanol extraction 1 ~ 3 time, filters; Filtering residue is used 50% washing with alcohol; Washing liquid merges with filtrating, and relative density was 1.10 ~ 1.30 extractum when concentrating under reduced pressure reclaimed ethanol to 60 ℃, promptly got.
2. the method for quality control of a stachydrine hydrochloride extractum is characterized in that, its operational approach is following:
Chromatographic condition and system suitability: adopt amino chromatographic column, with Yi Jing ︰ water by volume=solution of 75:25 mixed preparing is mobile phase, the detection wavelength is 198nm;
The preparation of reference substance solution: it is an amount of to get the stachydrine hydrochloride reference substance, and precision steelyard is fixed, adds the solution that methanol is processed the hydrochloric stachydrine 100 μ g of 1ml, as reference substance solution;
Supply the preparation of examination device solution: get stachydrine hydrochloride extractum 0.1g, precision steelyard is fixed, puts in the 50ml measuring bottle, and it is an amount of to add ethanol, and supersound process, shakes up to scale with ethanol dilution, filters, and gets this filtrating, as need testing solution;
Algoscopy: accurate respectively above-mentioned reference substance and each 20 μ l of need testing solution of drawing, inject high performance liquid chromatograph, according to high effective liquid chromatography for measuring, promptly get.
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| CN2012103605312A CN102836207A (en) | 2012-09-25 | 2012-09-25 | Preparation process of hydrochloric acid stachydrine extract and quality control method thereof |
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| CN2012103605312A CN102836207A (en) | 2012-09-25 | 2012-09-25 | Preparation process of hydrochloric acid stachydrine extract and quality control method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105911188A (en) * | 2016-04-25 | 2016-08-31 | 广西壮族自治区梧州食品药品检验所 | Method for rapid extraction-liquid chromatography-mass spectrometry tandem detection of content of stachydrine hydrochloride in Fukangning tablets |
| CN105911187A (en) * | 2016-04-25 | 2016-08-31 | 广西壮族自治区梧州食品药品检验所 | Method for liquid chromatography-mass spectrometry tandem detection of content of stachydrine hydrochloride in Fukangning tablets |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1833675A (en) * | 2006-01-05 | 2006-09-20 | 北京勃然制药有限公司 | Motherwort wort drip pills and prepn. method |
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2012
- 2012-09-25 CN CN2012103605312A patent/CN102836207A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1833675A (en) * | 2006-01-05 | 2006-09-20 | 北京勃然制药有限公司 | Motherwort wort drip pills and prepn. method |
Non-Patent Citations (1)
| Title |
|---|
| 张韵等: "HPLC法测定安坤益母草片中盐酸水苏碱的含量", 《广东药学院学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105911188A (en) * | 2016-04-25 | 2016-08-31 | 广西壮族自治区梧州食品药品检验所 | Method for rapid extraction-liquid chromatography-mass spectrometry tandem detection of content of stachydrine hydrochloride in Fukangning tablets |
| CN105911187A (en) * | 2016-04-25 | 2016-08-31 | 广西壮族自治区梧州食品药品检验所 | Method for liquid chromatography-mass spectrometry tandem detection of content of stachydrine hydrochloride in Fukangning tablets |
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Application publication date: 20121226 |