CN101361781A - Fingerprint checking method of gadol injection - Google Patents
Fingerprint checking method of gadol injection Download PDFInfo
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- CN101361781A CN101361781A CNA2008103001509A CN200810300150A CN101361781A CN 101361781 A CN101361781 A CN 101361781A CN A2008103001509 A CNA2008103001509 A CN A2008103001509A CN 200810300150 A CN200810300150 A CN 200810300150A CN 101361781 A CN101361781 A CN 101361781A
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Abstract
The invention relates to a quality inspection method for traditional Chinese medicine preparations, in particular to a fingerprint inspection method of integripetal rhodiola herb injection. The method comprises the steps of: (1) establishing the standard fingerprint of the integripetal rhodiola herb injection; (2) establishing the fingerprints of integripetal rhodiola herb injection samples; and (3) making a comparison between the fingerprints of the integripetal rhodiola herb injection samples and the standard fingerprint of the integripetal rhodiola herb injection and selecting a sample that meets the requirements of the standard fingerprint of the integripetal rhodiola herb injection. The method can qualitatively determine the major ingredients of the integripetal rhodiola herb injection and establish the proportion relationship between active ingredients and inactive ingredients in the injection so as to ensure the drug quality and the therapeutic effect of the integripetal rhodiola herb injection, effectively and reliably represent the product quality of the integripetal rhodiola herb injection and provide a new comparing standard for completely and correctly evaluating the quality of the integripetal rhodiola herb injection.
Description
Technical field
The present invention relates to a kind of detection method for quality of Chinese medicine preparation, specifically is the fingerprint checking method of gadol injection.
Background technology
In prior art, gadol injection is the patented product that Tonghua Yusheng Medicine Co., Ltd. produces without competition, the accurate word Z20060361 of traditional Chinese medicines.Composition: rhodiola kirilowii Regel.Function: set upright QI invigorating, blood circulation promoting and blood stasis dispelling, coronary circulation-promoting pain-relieving.Cure mainly: be used for the angina pectoris card and belong to the type of obstruction of heart-blood obstruction of qi in the chest and cardialgia.Disease is seen stabbing pain over the chest or angor, and time ends when doing, and localized pain is gone into Night Watch very, or palpitation and uneasiness, shortness of breath and fatigue, and purplish tongue, or ecchymosis is arranged; Deep and hesitant pulse etc.The quality of general Chinese medicine injection and curative effect be the content by can surveying composition in the medicinal liquid and to meet national injection standard just passable mainly, but exist different medical materials to contain the situation of same effective ingredient, therefore probably substitute another kind of medical material and improve content with different medical materials, may introduce new impurity and can not determine factor like this, give that medicine is clinical to bring very big risk.Because different medical materials all has different content composition and characteristic, fingerprint as the people, so the finger printing of the injection that different medicinal substances extracts is mixed with is just different, and has specificity, if added other medicinal substances extracts in this injection, the quantity at finger printing peak and peak area etc. all can change, and to make the finger printing of injection be very necessary so formulate single medical material, can check out whether this injection has added other medical materials in crude drug.
Summary of the invention
The purpose of this invention is to provide a kind of detection method and check the fingerprint checking method of gadol injection more reliably.
Technical solution of the present invention is: the fingerprint checking method of gadol injection comprises the steps:
(1) sets up the gadol injection standard finger-print
The preparation of a, need testing solution
Precision is measured gadol injection 2ml, puts in the 10ml measuring bottle, adds water for injection and is diluted to scale, shake up, extract 3 times, each 5ml with water saturated n-butyl alcohol jolting, merge n-butyl alcohol liquid, evaporate to dryness, residue add the dissolving of injection water, are transferred in the 5ml measuring bottle, be diluted to scale with water for injection, 0.45 μ m filtering with microporous membrane is got subsequent filtrate, promptly;
The preparation of b, standard solution
It is an amount of that precision takes by weighing the rhodioside reference substance, adds the dissolving of injection water, makes the solution that every 1ml contains the 0.05mg rhodioside;
C, chromatographic condition
Adopt F door Phenomenex chromatography post, mobile phase is 0.07% phosphoric acid solution, acetonitrile-methanol (volume ratio 1:1); Detect wavelength: 278nm; Column temperature: 30 ℃, carry out gradient elution;
D, mensuration
Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and make the gadol injection standard finger-print;
Described gadol injection standard finger-print is 10 batches of gadol injections to be carried out finger printing detect, and determines that 18 repeatability and relative retention time are total peak in the peak preferably, is the S peak with the corresponding peak of reference substance chromatographic peak in the test sample finger printing, the relative retention time at 18 total peaks and S peak is successively: 0.15 ± 10%, 0.20 ± 10%, 0.97 ± 10%, 1.18 ± 10%, 1.31 ± 10%, 1.42 ± 10%, 1.51 ± 10%, 1.61 ± 10%, 1.85 ± 10%, 2.01 ± 10%, 2.12 ± 10%, 2.33 ± 10%, 2.44 ± 10%, 2.62 ± 10%, 2.82 ± 10%, 2.91 ± 10%, 2.99 ± 10%, 3.07 ± 10%; Non-total peak area sum must not surpass 15% of total peak area;
(2) set up the finger printing of gadol injection sample to be measured with the identical method of step (1);
(3) gadol injection sample finger printing and the gadol injection standard finger-print that step (2) is obtained compares, and screening meets the sample of gadol injection standard finger-print requirement.
Advantage of the present invention is: 1, the HPCL finger printing of setting up with gadol injection is being represented the most of active component of Radix Rhodiolae, determine the main component of gadol injection qualitatively, set up the proportionate relationship of effective ingredient and non-active ingredients in this injection, with drug quality and the curative effect of guaranteeing gadol injection, can effectively, reliably characterize the product quality of gadol injection, for complete, accurately estimate the gadol injection quality new reference standard be provided.2, can check out that whether this gadol injection has added other medical material in crude drug, help the discriminating of authenticity of products.3, this method has characteristics easy, stable, favorable reproducibility, helps improving checkability.
Below in conjunction with embodiment the present invention is described in further detail.
Description of drawings
Fig. 1 is the gadol injection standard finger-print;
Fig. 2 is first sample finger printing of gadol injection;
Fig. 3 is the gadol injection second batch sample finger printing;
Fig. 4 is gadol injection the 3rd a batch sample finger printing.
The specific embodiment
Embodiment 1: the standard finger-print of gadol injection
The standard finger-print of gadol injection is set up and is comprised the steps:
The preparation of a, need testing solution
Precision is measured gadol injection 2ml, puts in the 10ml measuring bottle, adds water for injection and is diluted to scale, shake up, extract 3 times, each 5ml with water saturated n-butyl alcohol jolting, merge n-butyl alcohol liquid, evaporate to dryness, residue add the dissolving of injection water, are transferred in the 5ml measuring bottle, be diluted to scale with water for injection, microporous filter membrane (0.45 μ m) filters, and gets subsequent filtrate, promptly.
The preparation of b, standard solution
It is an amount of that precision takes by weighing the rhodioside reference substance, adds the dissolving of injection water, makes the solution that every 1ml contains the 0.05mg rhodioside
C, chromatographic condition
Chromatographic column: F door Phenomenex carbon 18 C18 (2) (4.60 * 150mm5 μ) chromatography post; Mobile phase is: A:0.07% phosphoric acid solution, B: acetonitrile-methanol (50:50); Detect wavelength: 278nm; Column temperature: 30 ℃; Detecting instrument: Tianjin, island SPD-10Avp, LC-10Avp.
According to the form below gradient elution: (table 1)
| Time (min) | Flow velocity (ml/min) | A(％) | B(％) |
| 0.01 | 0.5 | 91 | 9 |
| 24 | 0.5 | 80 | 20 |
| 42 | 0.7 | 78 | 22 |
| 60 | 1.0 | 70 | 30 |
| 60.01 | 1.0 | 91 | 9 |
| 75 | 1.0 | 91 | 9 |
| 75 | Stop |
D, algoscopy
Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure.
E, formulation gadol injection standard finger-print
Press the said determination method, 10 batches of gadol injections are carried out finger printing detect.Determine in 10 batches of collection of illustrative plates that 18 repeatability and relative retention time are total peak in the peak preferably, be the S peak with the corresponding peak of reference substance chromatographic peak in the test sample finger printing, the relative retention time (table 2) at 18 total peaks and S peak, non-total peak area and the long-pending ratio (table 3) of total front cover.
18 total peak relative retention time tables of gadol injection finger printing (table 2)
| Sample peak number | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | Sample 7 | Sample 8 | Sample 9 | Sample 10 | RSD％ |
| 1 | 0.15 | 0.15 | 0.15 | 0.15 | 0.16 | .015 | 0.16 | 0.15 | 0.15 | 0.16 | 2.22 |
| 2 | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 | 0.21 | 1.70 |
| 3 | 0.97 | 0.97 | 0.96 | 0.97 | 0.97 | 0.97 | 0.97 | 0.97 | 0.96 | 0.97 | 0.49 |
| 4 | 1.17 | 1.18 | 1.18 | 1.18 | 1.18 | 1.18 | 1.18 | 1.18 | 1.18 | 1.17 | 0.28 |
| 5 | 1.31 | 1.31 | 1.31 | 1.30 | 1.31 | 1.31 | 1.31 | 1.31 | 1.31 | 1.31 | 0.25 |
| 6 | 1.42 | 1.43 | 1.42 | 1.42 | 1.41 | 1.42 | 1.41 | 1.42 | 1.42 | 1.41 | 0.62 |
| 7 | 1.51 | 1.52 | 1.51 | 1.51 | 1.51 | 1.51 | 1.51 | 1.51 | 1.51 | 1.51 | 0.31 |
| 8 | 1.61 | 1.61 | 1.62 | 1.60 | 1.60 | 1.60 | 1.67 | 1.60 | 1.60 | 1.66 | 0.69 |
| 9 | 1.84 | 1.84 | 1.86 | 1.87 | 1.86 | 1.86 | 1.90 | 1.86 | 1.83 | 1.86 | 0.93 |
| 10 | 2.01 | 2.02 | 2.00 | 2.02 | 2.01 | 2.00 | 2.00 | 2.00 | 2.01 | 2.00 | 0.41 |
| 11 | 2.12 | 2.13 | 2.11 | 2.12 | 2.11 | 2.11 | 2.11 | 2.11 | 2.11 | 2.11 | 0.42 |
| 12 | 2.32 | 2.34 | 2.33 | 2.34 | 2.33 | 2.32 | 2.32 | 2.32 | 2.33 | 2.32 | 0.35 |
| 13 | 2.40 | 2.45 | 2.44 | 2.46 | 2.43 | 2.43 | 2.42 | 2.43 | 2.44 | 2.43 | 0.72 |
| 14 | 2.58 | 2.63 | 2.61 | 2.64 | 2.61 | 2.61 | 2.61 | 2.61 | 2.62 | 2.61 | 0.69 |
| 15 | 2.77 | 2.84 | 2.80 | 2.84 | 2.80 | 2.81 | 2.80 | 2.81 | 2.82 | 2.80 | 0.81 |
| 16 | 2.86 | 2.94 | 2.90 | 2.93 | 2.89 | 2.90 | 2.89 | 2.90 | 2.92 | 2.89 | 0.63 |
| 17 | 2.95 | 3.02 | 2.98 | 3.01 | 2.97 | 2.98 | 2.97 | 2.98 | 3.00 | 2.97 | 0.72 |
| 18 | 3.05 | 3.11 | 3.07 | 3.08 | 3.05 | 3.05 | 3.04 | 3.05 | 3.07 | 3.04 | 0.64 |
Non-total peak area and the long-pending ratio (table 3) of total front cover.
| Sample ratio | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | Sample 7 | Sample 8 | Sample 9 | Sample 10 |
| Non-total peak area | 14.6 | 14.4 | 12.2 | 14.1 | 13.6 | 10.8 | 13.2 | 12.7 | 13.3 | 9.5 |
Make the standard finger-print (referring to Fig. 1) of gadol injection according to above-mentioned data statistic
The gadol injection standard finger-print should meet the following requirements:
The test sample finger printing is similar to standard finger-print; Finger printing should have 18 total peaks; Relative retention time: 0.15 ± 10% (1), 0.20 ± 10% (2), 0.97 ± 10% (3), 1.18 ± 10% (4), 1.31 ± 10% (5), 1.42 ± 10% (6), 1.51 ± 10% (7), 1.61 ± 10% (8), 1.85 ± 10% (9), 2.01 ± 10% (10), 2.12 ± 10% (11), 2.33 ± 10% (12), 2.44 ± 10% (13), 2.62 ± 10% (14), 2.82 ± 10% (15), 2.91 ± 10% (16), 2.99 ± 10% (17), 3.07 ± 10% (18).Non-total peak area sum must not be crossed 15% of total peak area.
Embodiment 2: the gadol injection Application of Fingerprint
3 batch samples of producing in batches are checked.Set up the sample finger printing by the standard finger-print method for building up, get Fig. 2,3,4 finger printing.Evaluation and algoscopy compare three batches of gadol injection finger printing and standard gadol injection finger printing, the test sample finger printing is similar to standard finger-print, the relative retention time at 18 total peaks of three batch samples and non-total peak area and total peak area ratio are added up, and all meet the requirement of gadol injection standard finger-print.The gadol injection standard finger-print can be used for checking the gadol injection of batch process, and has specificity.
Claims (1)
- The fingerprint checking method of [claim 1] a kind of gadol injection is characterized in that comprising the steps: that (1) set up the gadol injection standard finger-print;The preparation of a, need testing solution:Precision is measured gadol injection 2ml, puts in the 10ml measuring bottle, adds water for injection and is diluted to scale, shake up, extract 3 times, each 5ml with water saturated n-butyl alcohol jolting, merge n-butyl alcohol liquid, evaporate to dryness, residue add the dissolving of injection water, are transferred in the 5ml measuring bottle, be diluted to scale with water for injection, 0.45 μ m filtering with microporous membrane is got subsequent filtrate, promptly;The preparation of b, standard solution:It is an amount of that precision takes by weighing the rhodioside reference substance, adds the dissolving of injection water, makes the solution that every 1ml contains the 0.05mg rhodioside;C, chromatographic condition:Adopt F door Phenomenex chromatography post, mobile phase is 0.07% phosphoric acid solution, acetonitrile-methanol volume ratio 1:1; Detect wavelength: 278nm; Column temperature: 30 ℃, carry out gradient elution;D, mensuration:Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and make the gadol injection standard finger-print;Described gadol injection standard finger-print is 10 batches of gadol injections to be carried out finger printing detect, and determines that 18 repeatability and relative retention time are total peak in the peak preferably, is the S peak with the corresponding peak of reference substance chromatographic peak in the test sample finger printing, the relative retention time at 18 total peaks and S peak is successively: 0.15 ± 10%, 0.20 ± 10%, 0.97 ± 10%, 1.18 ± 10%, 1.31 ± 10%, 1.42 ± 10%, 1.51 ± 10%, 1.61 ± 10%, 1.85 ± 10%, 2.01 ± 10%, 2.12 ± 10%, 2.33 ± 10%, 2.44 ± 10%, 2.62 ± 10%, 2.82 ± 10%, 2.91 ± 10%, 2.99 ± 10%, 3.07 ± 10%; Non-total peak area sum must not surpass 15% of total peak area;(2) set up the finger printing of gadol injection sample to be measured with the identical method of step (1);(3) gadol injection sample finger printing and the gadol injection standard finger-print that step (2) is obtained compares, and screening meets the sample of gadol injection standard finger-print requirement.
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| CNA2008103001509A CN101361781A (en) | 2008-01-18 | 2008-01-18 | Fingerprint checking method of gadol injection |
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| CNA2008103001509A CN101361781A (en) | 2008-01-18 | 2008-01-18 | Fingerprint checking method of gadol injection |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091118A (en) * | 2010-03-09 | 2011-06-15 | 成都中医药大学 | Quality detection method for rhodiola crenulata |
| CN102692464A (en) * | 2012-06-15 | 2012-09-26 | 通化玉圣药业股份有限公司 | Rhodiola rosea injection fingerprint spectrum check method |
| CN104435057A (en) * | 2014-12-19 | 2015-03-25 | 通化玉圣药业有限公司 | Preparation method of rhodiola rosea injection by low-temperature decarbonization |
| CN107543889A (en) * | 2016-06-28 | 2018-01-05 | 江苏康缘药业股份有限公司 | A kind of rhodiola kirilowii Regel capsule fingerprint pattern and its construction method |
| CN110716000A (en) * | 2019-11-18 | 2020-01-21 | 吉林大学 | Method for measuring content of p-hydroxyphenylacetic acid in rhodiola crenulata injection |
-
2008
- 2008-01-18 CN CNA2008103001509A patent/CN101361781A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091118A (en) * | 2010-03-09 | 2011-06-15 | 成都中医药大学 | Quality detection method for rhodiola crenulata |
| CN102091118B (en) * | 2010-03-09 | 2012-07-25 | 成都中医药大学 | Quality detection method for rhodiola crenulata |
| CN102692464A (en) * | 2012-06-15 | 2012-09-26 | 通化玉圣药业股份有限公司 | Rhodiola rosea injection fingerprint spectrum check method |
| CN104435057A (en) * | 2014-12-19 | 2015-03-25 | 通化玉圣药业有限公司 | Preparation method of rhodiola rosea injection by low-temperature decarbonization |
| CN107543889A (en) * | 2016-06-28 | 2018-01-05 | 江苏康缘药业股份有限公司 | A kind of rhodiola kirilowii Regel capsule fingerprint pattern and its construction method |
| CN107543889B (en) * | 2016-06-28 | 2019-02-22 | 江苏康缘药业股份有限公司 | A kind of rhodiola kirilowii Regel capsule fingerprint pattern and its construction method |
| CN110716000A (en) * | 2019-11-18 | 2020-01-21 | 吉林大学 | Method for measuring content of p-hydroxyphenylacetic acid in rhodiola crenulata injection |
| CN110716000B (en) * | 2019-11-18 | 2021-12-10 | 吉林大学 | Method for measuring content of p-hydroxyphenylacetic acid in rhodiola crenulata injection |
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Open date: 20090211 |