CN104597201A - Method for detecting scutellarin content - Google Patents
Method for detecting scutellarin content Download PDFInfo
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- CN104597201A CN104597201A CN201310526940.XA CN201310526940A CN104597201A CN 104597201 A CN104597201 A CN 104597201A CN 201310526940 A CN201310526940 A CN 201310526940A CN 104597201 A CN104597201 A CN 104597201A
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- acid solution
- lamp
- dish flower
- flower acetic
- alkali lye
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Abstract
The invention relates to the field of analytical chemistry and discloses a method for detecting scutellarin content. The method comprises the following steps of weighing a scutellarin-containing product to be detected, completely dissolving the product in alkali lye, carrying out titration until a reaction terminal point by an acid solution, recording a consumed volume of a first acid solution, taking alkali lye with a volume the same as that of the used alkali lye, carrying out titration until a reaction terminal point by the acid solution, recording a consumed volume of a second acid solution, and carrying out calculation by the two consumed volumes according to a formula. The method can detect scutellarin content by an alkali residual titration method, is free of an expensive scutellarin contrast, is simple, fast and accurate, has good reappearance, greatly reduces a detection cost and is especially suitable for semi-finished product quantitative analysis and low-added value breviscapinun preparation analysis.
Description
Technical field
The present invention relates to analytical chemistry field, relate to a kind of method detecting lamp-dish flower acetic content in particular.
Background technology
Fleabane flower has another name called erigeron breviscapus, and because flower is like oil lamp, root is gained the name like the root of Chinese wild ginger, is the herb of the short booth bitter fleabane of composite family bitter fleabane platymiscium [Erigeron breviscapus (vant.) Hand.-Mazz.].This medicinal material head is loaded in " the southern regions of the Yunnan Province book on Chinese herbal medicine ", has recorded " Chinese Pharmacopoeia 2005 version, Yunnan is among the people is usually used in treatment traumatic injury, rheumatalgia pain, toothache, stomachache, flu etc.Twentieth century seventies, chronic archnoiditis and sequelae thereof had good therapeutic effect, and also have certain curative effect to rheumatism, coronary heart disease through clinical verification to hypertension, cerebral hemorrhage, cerebral thrombosis, cerebral embolism polyneuritis.Medical research shows that the main active of erigeron breviscapus for treating cardiovascular and cerebrovascular disease is Breviscapinun (Breviscapine), and Breviscapinun is mainly containing lamp-dish flower acetic (Scutellarin), has another name called scutellarin, molecular formula C
21h
18o
12, molecular weight is 462.37.
At present, Breviscapinun drug products mainly contains Breviscapine sustained-release tablets, breviscapine drop pills, erigeron breviscapus dispersion tablet etc.In prior art, the impact because of preparation technology makes lamp-dish flower acetic content between each batch of Breviscapinun drug products occur fluctuation, and the content for Accurate Determining lamp-dish flower acetic is the important indicator weighing Breviscapinun drug product quality.
The quality standard of Breviscapinun has been recorded " Chinese Pharmacopoeia " version in 2010, and adopt HPLC external standard reference substance method to detect the content of lamp-dish flower acetic (or scutellarin), the method is exclusive, and accurately, but it is high to there is testing cost, the deficiency that sense cycle is long.Also the document had take rutin as reference substance after adopting and Breviscapinun and tri-chlorination chlorine being developed the color, and ultraviolet spectrophotometry detects general flavone, but the method specificity is poor, detects inaccurate.
Summary of the invention
In view of this, the object of this invention is to provide a kind of method of easy, cost is low and accuracy is high detection lamp-dish flower acetic content.
For achieving the above object, the invention provides following technical scheme:
Detect a method for lamp-dish flower acetic content, comprising:
Step 1, take product to be tested containing lamp-dish flower acetic, dissolve completely with alkali lye, be then titrated to reaction end by acid solution, record the first acid solution and consume volume;
Step 2, get the described alkali lye of step 1 same volume, be titrated to reaction end by acid solution described in step 1, record the second acid solution and consume volume;
Step 3, namely obtain lamp-dish flower acetic percentage composition according to following formulae discovery:
The present invention adopts the molten acid of alkali to sink principle, dissolves lamp-dish flower acetic with alkali lye, with the alkali that acidometric titration is unnecessary, according to the volume of the volume computing alkali lye real reaction that acid solution titration consumes, thus calculates lamp-dish flower acetic content.
Add alkali and dissolve lamp-dish flower acetic:
R-COOH(lamp-dish flower acetic)+OH
-→ R-COO
-(lamp-dish flower acetic carboxylate)+H
2o
For the determination of reaction end, the present invention preferably adopts potentiometric titrimeter to judge, also can adopt other suitable determination methods in addition.
Wherein, as preferably, described alkali lye is sodium hydrate aqueous solution or potassium hydroxide aqueous solution, it is further preferred that described alkali lye is sodium hydrate aqueous solution or the potassium hydroxide aqueous solution of volumetric molar concentration 0.01mol/L-0.1mol/L
As preferably, the volumetric molar concentration of described alkali lye is 0.01mol/L-0.1mol/L.
As preferably, described acid solution is hydrochloric acid or sulfuric acid, it is further preferred that described acid solution is volumetric molar concentration 0.01mol/L-0.1mol/L hydrochloric acid or sulfuric acid.
As preferably, the volumetric molar concentration of described acid solution is 0.01mol/L-0.1mol/L.
The method of the invention can detect the product containing lamp-dish flower acetic, particularly Breviscapine, and described Breviscapine is preferably from Breviscapine sustained-release tablets, breviscapine drop pills or erigeron breviscapus dispersion tablet.
The method of the invention and HPLC method adopt the product to be tested in identical source to carry out the detection of lamp-dish flower acetic content, and result shows two kinds of method data consistents, does not have significant difference.The method of the invention is through checking simultaneously, good in 4mg/mL-40mg/mL scope internal linear relation, and the RSD% of repeatability and precision test is respectively 1.17% and 0.24%, and the recovery is 98.8%.
From above technical scheme, the present invention adopts buffuer excess titration method and measures lamp-dish flower acetic content, have not relate to and use expensive lamp-dish flower acetic reference substance, method is easy, fast, accurately, favorable reproducibility, the advantage that testing cost reduces greatly, is especially applicable to semi-manufacture quantitative test and low value-added Breviscapine analysis.
Embodiment
The invention discloses a kind of method detecting lamp-dish flower acetic content, those skilled in the art can use for reference present disclosure, and suitable improving technique parameter realizes.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are all deemed to be included in the present invention.Method of the present invention is described by preferred embodiment, related personnel obviously can not depart from content of the present invention, spirit and scope methods and applications as herein described are changed or suitably change with combination, realize and apply the technology of the present invention.
Below in conjunction with embodiment, set forth the present invention further.
Embodiment 1: the present invention detects the method for lamp-dish flower acetic content
Take the product to be tested containing lamp-dish flower acetic, dissolve completely with the sodium hydrate aqueous solution of 0.1mol/L, then use the HCI of 0.1mol/L, Switzerland Meton potentiometric titrimeter Indicator Reaction terminal, records the first acid solution (hydrochloric acid) and consumes volume;
Get the sodium hydrate aqueous solution of the 0.1mol/L of above-mentioned same volume, with the HCI of 0.1mol/L to reaction end, record the second acid solution (hydrochloric acid) and consume volume;
Namely lamp-dish flower acetic percentage composition is obtained according to following formulae discovery:
Embodiment 2: the present invention detects the method for lamp-dish flower acetic content
Take the product to be tested containing lamp-dish flower acetic, dissolve completely with the potassium hydroxide aqueous solution of 0.01mol/L, then use the sulfuric acid titration of 0.01mol/L, Switzerland Meton potentiometric titrimeter Indicator Reaction terminal, records the first acid solution (sulfuric acid) and consumes volume;
Get the potassium hydroxide aqueous solution of the 0.01mol/L of above-mentioned same volume, be titrated to reaction end with the sulfuric acid of 0.01mol/L, record the second acid solution (sulfuric acid) and consume volume;
Namely lamp-dish flower acetic percentage composition is obtained according to following formulae discovery:
Embodiment 3: the present invention detects the method for lamp-dish flower acetic content
Take the product to be tested containing lamp-dish flower acetic, dissolve completely with the sodium hydrate aqueous solution of 0.05mol/L, then use the phosphoric acid titration of 0.05mol/L, Switzerland Meton potentiometric titrimeter Indicator Reaction terminal, records the first acid solution (phosphoric acid) and consumes volume;
Get the sodium hydrate aqueous solution of the 0.05mol/L of above-mentioned same volume, be titrated to reaction end with the phosphoric acid of 0.05mol/L, record the second acid solution (phosphoric acid) and consume volume;
Namely lamp-dish flower acetic percentage composition is obtained according to following formulae discovery:
Embodiment 4: measure lamp-dish flower acetic content in commercially available Breviscapine sustained-release tablets
1, articles for use are detected
Product to be tested: commercially available Breviscapine sustained-release tablets, Kunming pharmacy group provides, lot number: 20061079, specification: calculate according to lamp-dish flower acetic: 60mg/ sheet.
Instrument and reagent reagent: water is water for injection; Hydrochloric acid, NaOH are AG; Natrium carbonicum calcinatum, Potassium Hydrogen Phthalate is reference level reagent; Container transfer pipet (25ml, 10ml, 5ml) used, volumetric flask (250ml), acid dropper (10ml) are all calibrated meets country one, goods of inferior quality standard.
Autopotentiometric titrator: Switzerland Metrohm autopotentiometric titrator, main frame is 888Titrando, 801stimer stirrer, 803Tistand titration platform.
2, detection method
Measure according to embodiment 1 method.Measurement result: every sheet is calculated as 61.7mg containing Breviscapinun by lamp-dish flower acetic.Indicate without significant difference with commercially available Breviscapine sustained-release tablets.
Embodiment 5: measure lamp-dish flower acetic content in commercially available breviscapine drop pills
1, articles for use are detected
Product to be tested: commercially available breviscapine drop pills, Kunming pharmacy group provides, lot number: 20121008, specification: calculate according to lamp-dish flower acetic: 4mg/ ball.
Instrument and reagent reagent: water is water for injection; Sulfuric acid, potassium hydroxide are AG; Natrium carbonicum calcinatum, Potassium Hydrogen Phthalate is reference level reagent; Container transfer pipet (25ml, 10ml, 5ml) used, volumetric flask (250ml), acid dropper (10ml) are all calibrated meets country one, goods of inferior quality standard.
Autopotentiometric titrator: Switzerland Metrohm autopotentiometric titrator, main frame is 888Titrando, 801stimer stirrer, 803Tistand titration platform.
2, detection method
Measure according to embodiment 2 method.Measurement result: every ball is calculated as 3.9mg containing Breviscapinun by lamp-dish flower acetic.Indicate without significant difference with commercially available breviscapine drop pills.
Embodiment 6: measure lamp-dish flower acetic content in commercially available erigeron breviscapus dispersion tablet
1, articles for use are detected
Product to be tested: commercially available erigeron breviscapus dispersion tablet, Kunming pharmacy group provides, lot number: 20110509, specification: calculate according to lamp-dish flower acetic: 40mg/ sheet.
Instrument and reagent reagent: water is water for injection; Sulfuric acid, potassium hydroxide are AG; Natrium carbonicum calcinatum, Potassium Hydrogen Phthalate is reference level reagent; Container transfer pipet (25ml, 10ml, 5ml) used, volumetric flask (250ml), acid dropper (10ml) are all calibrated meets country one, goods of inferior quality standard.
Autopotentiometric titrator: Switzerland Metrohm autopotentiometric titrator, main frame is 888Titrando, 801stimer stirrer, 803Tistand titration platform.
2, detection method
Measure according to embodiment 2 method.Measurement result: every sheet is calculated as 40.5mg containing Breviscapinun by lamp-dish flower acetic.Indicate without significant difference with commercially available erigeron breviscapus dispersion tablet.
Embodiment 7: detect with the contrast of HPLC
Detection method: the embodiment of the present invention 2 detection method and " Chinese Pharmacopoeia " version in 2010 high performance liquid chromatography recorded.
Product to be tested: Breviscapine sustained-release tablets, by Kunming, pharmacy group provides, lot number: HB201111001,20111226,20120517.
Lamp-dish flower acetic content detection the results are shown in Table 1.
Table 1 contrasts testing result
| Lot number | Embodiment 2 testing result | HPLC testing result |
| HB201111001 | 98.52% | 98.57% |
| 20111226 | 97.90% | 98.74% |
| 20120517 | 97.96% | 98.25% |
As seen from the above table, the lamp-dish flower acetic content detected according to the embodiment of the present invention 2 detection method and the result no significant difference adopting HPLC method to detect, have higher accuracy.
Embodiment 8: the method for the invention specificity detects
Detection method: the embodiment of the present invention 1 detection method.
Product to be tested: Breviscapine sustained-release tablets and auxiliary material thereof, by Kunming, pharmacy group provides, lot number: HB201111001,20111226.
Testing result is in table 2.
Table 2 specificity testing result
| First acid solution consumes volume | |
| HB201111001 | 14.8737mL |
| 20111226 | 14.6402mL |
| Breviscapine slow release auxiliary material | 24.6060mL |
| Blank (namely the second acid solution consumes volume) | 24.3579mL |
As can be seen from Table 2, the auxiliary material of Breviscapine sustained-release tablets does not consume alkali lye, thus acid solution consumes volume and does not add the second acid solution consumption volume (blank) no significant difference of any product to be tested, show that the detection specificity of the method for the invention is strong, product auxiliary material does not disturb the mensuration of lamp-dish flower acetic content.
Embodiment 9: the method for the invention linearity detects
(Kunming pharmacy group provides to get Breviscapinun, lot number is the Breviscapine sustained-release tablets of HB20111001) be about 0.1g containing being equivalent to lamp-dish flower acetic, 0.14g, 0.2g, 0.25g, 0.3g, 0.35g, 0.4g, 0.5g, 0.6g, 0.7g, 0.8g, the product to be tested of 1.0g to put in small beaker 12 parts, accurately weighed, be numbered 1 ~ 12 respectively, precision measures sodium hydrate aqueous solution 25ml makes it dissolve, with the Breviscapinun of HCI liquid stepwise titration variable concentrations, with the volume (V) that sodium hydrate aqueous solution consumes, lamp-dish flower acetic concentration (C) is returned, and draw typical curve.
Lamp-dish flower acetic is good in 4mg/mL-40mg/mL scope internal linear relation, and equation of linear regression is: C (SCU)=17.99 × V (NaOH)+0.4334, r=0.9999.
Embodiment 10: the method for the invention repeatability detects
Get Breviscapinun (Kunming pharmacy group provides, and lot number is the Breviscapine sustained-release tablets of 20061079) sustained release tablets sample and to put in small beaker 6 parts, accurately weighed, detect according to embodiment 1 method, the results are shown in Table 3.
Table 3 repeatability detects
| Measure number of times | 1 | 2 | 3 | 4 | 5 | 6 | RSD% |
| Lamp-dish flower acetic content % | 93.76 | 94.71 | 95.1 | 93.85 | 94.96 | 96.84 | 1.17 |
As shown in Table 3, the RSD% that the method for the invention detects the result of same sample is 1.17%, and far below 3% of standard regulation, repeatability better.
Embodiment 11: the method for the invention precision detects
Get same Breviscapine sustained-release tablets product to be tested, dividing equally is 6 parts, accurately weighed in 250ml volumetric flask, hydro-oxidation sodium vs (0.1mol/L) is fixed molten, and precision measures 25ml, with HCI liquid (0.1mol/L) titration, potentiometric titrimeter directing terminal, the results are shown in Table 4.
Table 4: Precision Experiment result
| Measure number of times | 1 | 2 | 3 | 4 | 5 | 6 | RSD% |
| First acid solution consumes volume (ml) | 15.37 | 15.42 | 15.37 | 15.37 | 15.30 | 15.36 | 0.24 |
Result shows, RSD% is all less than 0.3%, and precision is better.
Embodiment 12: the detection method recovery detects
Get with totally 12 parts, a collection of product to be tested powder, be numbered 1 ~ 12 respectively.Wherein, 1st ~ 3 parts do not add lamp-dish flower acetic reference substance, and 4th ~ 6 parts add lamp-dish flower acetic reference substance 0.15g, 7th ~ 9 parts add lamp-dish flower acetic reference substance 0.25g, and 10th ~ 12 parts add lamp-dish flower acetic reference substance 0.35g, detect by embodiment 1 method, calculate the recovery, data result is in table 5.
Table 5 lamp-dish flower acetic recovery test result
Recovery test shows, average recovery rate is greater than 98.0%, with the method for the invention can by containing lamp-dish flower acetic product to be tested in lamp-dish flower acetic Accurate Determining out.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. detect a method for lamp-dish flower acetic content, it is characterized in that, comprising:
Step 1, take product to be tested containing lamp-dish flower acetic, dissolve completely with alkali lye, be then titrated to reaction end by acid solution, record the first acid solution and consume volume;
Step 2, get the described alkali lye of step 1 same volume, be titrated to reaction end by acid solution described in step 1, record the second acid solution and consume volume;
Step 3, namely obtain lamp-dish flower acetic percentage composition according to following formulae discovery:
2. method according to claim 1, it is characterized in that, described alkali lye is sodium hydrate aqueous solution or potassium hydroxide aqueous solution.
3. method according to claim 1, it is characterized in that, the volumetric molar concentration of described alkali lye is 0.01mol/L-0.1mol/L.
4. method according to claim 1, it is characterized in that, described acid solution is hydrochloric acid or sulfuric acid.
5. method according to claim 1, it is characterized in that, the volumetric molar concentration of described acid solution is 0.01mol/L-0.1mol/L.
6. method according to claim 1, is characterized in that, the described product to be tested containing lamp-dish flower acetic is Breviscapine.
7. method according to claim 6, it is characterized in that, described Breviscapine is Breviscapine sustained-release tablets, breviscapine drop pills or erigeron breviscapus dispersion tablet.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1857357A (en) * | 2006-03-09 | 2006-11-08 | 南昌弘益科技有限公司 | Quality control method for disolubility of solid oral breviscapine preparation |
| CN102023188A (en) * | 2009-09-16 | 2011-04-20 | 昆明制药集团股份有限公司 | Quality control method of scutellarin |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1857357A (en) * | 2006-03-09 | 2006-11-08 | 南昌弘益科技有限公司 | Quality control method for disolubility of solid oral breviscapine preparation |
| CN102023188A (en) * | 2009-09-16 | 2011-04-20 | 昆明制药集团股份有限公司 | Quality control method of scutellarin |
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