CN104535690B - Method for measuring content of cinnarizine in cinnarizine solid preparation - Google Patents
Method for measuring content of cinnarizine in cinnarizine solid preparation Download PDFInfo
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- CN104535690B CN104535690B CN201510016210.4A CN201510016210A CN104535690B CN 104535690 B CN104535690 B CN 104535690B CN 201510016210 A CN201510016210 A CN 201510016210A CN 104535690 B CN104535690 B CN 104535690B
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Abstract
The invention relates to the technical field of medicine and pharmacy, in particular to a method for measuring the content of cinnarizine in a cinnarizine solid preparation. An efficient liquid phase chromatography is adopted, methanol directly serves as a mobile phase to measure the content of the cinnarizine in the cinnarizine solid preparation or in a content of the cinnarizine solid preparation, methodology validation is conducted on the method, and compared with an existing method for measuring the content of the cinnarizine through existing detection technologies, the method has the advantages of being efficient, convenient, accurate and the like. Meanwhile, more errors caused by manual operation are reduced, and detection accuracy is improved.
Description
Technical field
The present invention relates to medical pharmaceutical technology field, measure Cinnarizine content in Cinnarizine solid preparation particularly to a kind of
Method.
Background technology
At present version pharmacopeia in 2010 is measured for Cinnarizine drug content and use perchloric acid titration method, tablet and capsule
Agent content measures version pharmacopeia in 2010 and uses ultraviolet spectrophotometry.Both detection method raw materials and preparation disunity
It is likely to result in and accomplishes that preparation may have certain content error with a collection of raw material, and the method anthropic factor is larger.
Content of the invention
The present invention provides a kind of method measuring Cinnarizine content in Cinnarizine solid preparation, in order to solve in prior art
Have such problems as that detection error is big, accuracy is not high.
A kind of method measuring Cinnarizine content in Cinnarizine solid preparation of the present invention includes detecting Cinnarizine master
The content of Cinnarizine in medicine, Cinnarizine tablet and Cinnarizine capsule contents composition granule, described Cinnarizine preparation adopts for our company
High speed wet granulation is independently produced.
For solving above-mentioned technical problem, the present invention adopts the following technical scheme that, in a kind of mensure Cinnarizine solid preparation
The method of Cinnarizine content, with Cinnarizine reference substance for comparison, with methanol as mobile phase, using high effective liquid chromatography for measuring osmanthus
The content of Cinnarizine in sharp piperazine solid preparation.
Specifically, with Cinnarizine reference substance for comparison, with methanol as mobile phase, using high performance liquid chromatography in 253nm
The content of Cinnarizine in Cinnarizine solid preparation is measured at wavelength.
More specifically, the detection method of described content is：
(1) chromatographic condition and its system suitability：Chromatographic column：C18 post 250 × 4.6mm；Mobile phase：Methanol；Flow velocity：0.8
～1.2ml/min；Detection wavelength：253nm；Sample size：10μl；40～50 DEG C of column temperature；System suitability：Number of theoretical plate presses osmanthus profit
Piperazine peak calculates and is not less than 1000；
(2) preparation of reference substance solution：Take Cinnarizine reference substance appropriate, accurately weighed, plus methanol is configured to every 1ml and contains osmanthus
The solution of sharp piperazine 1.3ug, obtains final product；
(3) preparation of need testing solution：Precision weighs Cinnarizine preparation or its content, is equivalent to Cinnarizine 13mg and (presses
Photo weight or ball weight and preparation specification 10mg are converted), weighed, put in 100ml measuring bottle, plus methanol dissolves and is diluted to quarter
Degree, shakes up；Precision measures 1ml, puts in 100ml measuring bottle, plus methanol, to scale, shakes up, and obtains final product；
(4) algoscopy：Precision measures reference substance solution and each 10 μ l of need testing solution respectively, injects high performance liquid chromatography
Instrument, measures Cinnarizine content；
Preferably, described flow velocity is 1.0ml/min.
Preferably, described column temperature is 45 DEG C.
Preferably, being formulated as of described reference substance solution：Take Cinnarizine reference substance 13mg, accurately weighed, put 100ml measuring bottle
In, plus methanol dissolves and is diluted to scale, shakes up；Precision measures 1ml, puts in 100ml measuring bottle, plus methanol to scale, shakes up, that is,
Obtain the solution that every 1ml contains Cinnarizine 1.3ug.
The present invention has the beneficial effect that：The method uses high performance liquid chromatography, directly with methanol as mobile phase；Efficiently,
Fast, accurately；Decrease the error of manual operation；Simultaneously can be for the formula of improvement Cinnarizine solid preparation and its to osmanthus in medicine
The assay of sharp piperazine provides important references.
Brief description
Fig. 1 is that the HPLC of Cinnarizine standard substance detects collection of illustrative plates；
Fig. 2 is Cinnarizine linear relationship chart and equation of linear regression.
Specific embodiment
With reference to Figure of description, the present invention and embodiment are described in further detail.
For guaranteeing the science of content assaying method of the present invention, reasonable, feasible, inventor has carried out a series of experimental study
And investigation.
First, reagent (being shown in Table 1)
Table 1
Note：Methanol used is chromatographically pure (Fisher company)
2nd, method and result
1st, chromatographic condition：Chromatographic column：C18 post 250 × 4.6mm；Mobile phase：Methanol；Flow velocity：1.0ml/min；Detection ripple
Long：253nm；Sample size：10μl；45 DEG C of column temperature.
2nd, drug content method for measuring checking in Cinnarizine solid preparation
2.1 test limits, quantitative limit
2.1.1 evaluation criterion
Test limit evaluation criterion：Signal to noise ratio is 3:1, relative standard deviation is not more than 10.0%.
Quantitative limit evaluation criterion：Signal to noise ratio about 10:1, relative standard deviation is not more than 10.0%.
2.1.2 test limit test liquid and quantitative limit test liquid are prepared
Storing solution：Take Cinnarizine reference substance about 13mg, accurately weighed, put in 100ml measuring bottle, plus methanol dissolves and is diluted to
Scale, shakes up, as storing solution.
Test limit test liquid：Storing solution is taken progressively to be diluted to 3 times of about baseline height.
Quantitative limit test liquid：Storing solution is taken progressively to be diluted to 10 times of about baseline height.
2.1.3 algoscopy
A, lucifuge operation, precision measures above-mentioned test limit test liquid and the limitation property each 10ug of test liquid, with signal to noise ratio 3:When 1
Injection high performance liquid chromatograph, determines that this concentration is minimal detectable concentration, by minimal detectable concentration continuous sample introduction 5 times, by " 1 color
Spectral condition " is measured, the peak area at Cinnarizine peak in record chromatogram, and result shows：The RSD value of peak area for 8.5% (see
Table 2), coincidence detection limits evaluation criterion.
Table 2 test limit result
B, lucifuge operation, precision measures above-mentioned quantitative limit test liquid and the limitation property each 10ug of test liquid, with signal to noise ratio 10:1
When inject high performance liquid chromatograph, determine that this concentration is minimal detectable concentration, by minimal detectable concentration continuous sample introduction 5 times, by " 1
Chromatographic condition " is measured, the peak area at Cinnarizine peak in record chromatogram, and result shows：The RSD value of peak area is
0.392054% (being shown in Table 3), meets limitation property evaluation criterion.
Table 3 limitation property result
2.2 it is linear
2.2.1 the preparation of test liquid
Test liquid storing solution：Precision weighs Cinnarizine reference substance about 20mg, puts in 100ml measuring bottle, plus methanol makes Cinnarizine
Dissolve, plus methanol dilution, to scale, shakes up；Precision measures 10ml, puts in 250ml measuring bottle, plus methanol dilution, to scale, shakes up,
Concentration is 8ug/ml, as test liquid storing solution.
Test liquid A：Precision measures test liquid storing solution 5.0ml, puts in 200ml measuring bottle, plus methanol dilution, to scale, shakes
Even；Precision measures 5.0ml, puts in 100ml measuring bottle, plus methanol dilution, to scale, shakes up, and concentration is 0.01ug/ml.
Test liquid B：Precision measures test liquid storing solution 1.0ml, puts in 25ml measuring bottle, plus methanol dilution, to scale, shakes up,
Concentration is 0.32ug/ml.
Test liquid C：Precision measures test liquid storing solution 2.0ml, puts in 25ml measuring bottle, plus methanol dilution, to scale, shakes up,
Concentration is 0.64ug/ml.
Test liquid D：Precision measures test liquid storing solution 3.0m, puts in 25ml measuring bottle, plus methanol dilution, to scale, shakes up
Even, concentration is 0.96ug/ml.
Test liquid E：Precision measures test liquid storing solution 4.0ml, puts in 25ml measuring bottle, plus methanol dissolves and is diluted to quarter
Degree, shakes up, and concentration is 1.28ug/ml.
Test liquid F：Precision measures test liquid storing solution 5.0ml, puts in 25ml measuring bottle, plus methanol dilution, to scale, shakes up,
Concentration is 1.60ug/ml.
Test liquid G：Precision measures test liquid storing solution 6.0ml, puts in 25ml measuring bottle, plus methanol dilution, to scale, shakes up,
Concentration is 1.92ug/ml.
Take above-mentioned test liquid A, B, C, D, E, F, G each 10ug injection chromatograph of liquid respectively, surveyed by " 1 chromatographic condition "
Fixed, record chromatogram, calculate correlation coefficient and linear equation (being shown in Table 4), with the amount (mg/mL) of Cinnarizine test liquid as abscissa
(X), peak area is vertical coordinate (Y), draws standard curve (see Fig. 2), and the regression equation obtaining Cinnarizine is y=32.425x-
0.02486, result shows：The content of Cinnarizine is in good linear relationship with peak area, can meet mensure and require.
Table 4 correlation coefficient and linear equation
2.3 accuracy, precision, specificity experiment
Evaluation criterion：The response rate >=70.0%；RSD9≤10.0%；RSD6≤2.0%.
Test liquid storing solution：Precision weighs Cinnarizine reference substance about 20mg, puts 100ml measuring bottle, plus methanol, shaking, makes osmanthus
Sharp piperazine dissolves, plus methanol dilution, to scale, shakes up, and concentration is 200ug/ml.
Test liquid 1：Precision measures storing solution 3.30ml, puts in 10ml measuring bottle, plus methanol dilution, to scale, shakes up, concentration
For 0.66ug/ml.
Test liquid 2：Precision measures storing solution 6.50ml, puts in 10ml measuring bottle, plus methanol dilution, to scale, shakes up, concentration
For 1.30ug/ml.
Test liquid 3：Precision measures storing solution 9.75ml, puts in 10ml measuring bottle, plus methanol dilution, to scale, shakes up, concentration
For 1.95ug/ml.
Contrast solution：Precision measures 1.0ml test liquid 2, puts in 100ml measuring bottle, plus methanol dilution, to scale, shakes up, dense
Spend for 0.03ug/ml.
Blank solution：Methanol solution, direct injected, noiseless near main peak.
Take above-mentioned test liquid 1, test liquid 2, test liquid 3, contrast solution, blank solution each 10ug injection chromatograph of liquid,
It is measured recording chromatogram by " 1, chromatographic condition ", the peak area at Cinnarizine peak in record chromatogram, result shows：Peak area
Average recovery rate be 89.2, RSD9 be 4.8%, show that the accuracy of the method is high, high-specificity, instrument precision is good
(being shown in Table 5).
Table 5 accuracy, precision, specificity experimental result
As can be seen that the method accuracy, precision, specificity all meet from above-mentioned each summary sheet and each detection data
Regulation, average recovery rate is 89.2%, RSD9 is 4.8%；Linearly dependent coefficient r=0.997；All conformance with standard.The method can
To apply to measure Cinnarizine content in Cinnarizine solid preparation (including Cinnarizine principal agent, Cinnarizine tablet, Cinnarizine capsule)
Practice examining, can for improve Cinnarizine solid preparation formula and its in medicine Cinnarizine assay provide important ginseng
Examine.
3rd, sample size detection
The Cinnarizine solid preparation precisely weighing the friendship everything Pharmaceutical different batches production of upper Hisense respectively (includes cinnarizine tablets
Agent and Cinnarizine capsule 's content), prepare need testing solution, respectively take 10ug to be measured recording chromatograph by " 1, chromatographic condition "
Figure, records peak area, calculates Cinnarizine content (being shown in Table 6) according to above-mentioned " 2.2 is linear " equation of linear regression.
Table 6 sample size detects
Embodiment 1
The mensure of Cinnarizine content in Cinnarizine tablet (upper Hisense friendship everything Pharmaceutical, 10mg)
(1) chromatographic condition：Chromatographic column：C18 post 250 × 4.6mm；Mobile phase：Methanol；Flow velocity：1.0ml/min；Detection ripple
Long：253nm；Sample size：10μl；45 DEG C of column temperature.
(2) contrast solution：Take Cinnarizine reference substance about 13mg, accurately weighed, put in 100ml measuring bottle, plus methanol dissolves simultaneously
It is diluted to scale, shake up；Precision measures 1ml, puts in 100ml measuring bottle, plus methanol to scale, shakes up, as contrast solution
(1.3ug/ml)；
(3) preparation of sample solution：Precision weighs Cinnarizine tablet, is approximately equivalent to Cinnarizine 13mg, weighed, puts 100ml
In measuring bottle, plus methanol dissolves and is diluted to scale, shakes up；Precision measures 1ml, puts in 100ml measuring bottle, plus methanol, to scale, shakes
Even, as sample solution；
(4) assay method：Precision measures above-mentioned contrast solution and each 10 μ l injection chromatograph of liquid of sample solution, records color
Spectrogram, measures, obtains final product.
Embodiment 2
The mensure of Cinnarizine content in Cinnarizine capsule content (upper Hisense friendship everything Pharmaceutical, 10mg)
(1) chromatographic condition：Chromatographic column：C18 post 250 × 4.6mm；Mobile phase：Methanol；Flow velocity：0.8ml/min；Detection ripple
Long：253nm；Sample size：10μl；40 DEG C of column temperature.
(2) contrast solution：Take Cinnarizine reference substance 13mg, accurately weighed, put in 100ml measuring bottle, plus methanol dissolves and dilute
Release to scale, shake up；Precision measures 1ml, puts in 100ml measuring bottle, plus methanol, to scale, shakes up, as contrast solution (1.3ug/
ml)；
(3) preparation of sample solution：Precision weighs Cinnarizine capsule preparations content, is equivalent to Cinnarizine 13mg, weighed,
Put in 100ml measuring bottle, plus methanol dissolves and is diluted to scale, shakes up；Precision measures 1ml, puts in 100ml measuring bottle, plus methanol is extremely
Scale, shakes up, as sample solution；
(4) assay method：Precision measures above-mentioned contrast solution and each 10 μ l injection chromatograph of liquid of sample solution, records color
Spectrogram, measures, obtains final product.
Embodiment 3
The survey of Cinnarizine content in principal agent raw material Cinnarizine (commercially available) of preparation Cinnarizine tablet and Cinnarizine capsule
Fixed
(1) chromatographic condition：Chromatographic column：C18 post 250 × 4.6mm；Mobile phase：Methanol；Flow velocity：1.2ml/min；Detection ripple
Long：253nm；Sample size：10μl；50 DEG C of column temperature.
(2) contrast solution：Take Cinnarizine reference substance 13mg, accurately weighed, put in 100ml measuring bottle, plus methanol dissolves and dilute
Release to scale, shake up；Precision measures 1ml, puts in 100ml measuring bottle, plus methanol, to scale, shakes up, as contrast solution (1.3ug/
ml)；
(3) preparation of sample solution：Precision weighs Cinnarizine raw material 13mg, weighed, puts in 100ml measuring bottle, plus methanol is molten
Solve and be diluted to scale, shake up；Precision measures 1ml, puts in 100ml measuring bottle, plus methanol to scale, shakes up, as sample solution；
(4) assay method：Precision measures above-mentioned contrast solution and each 10 μ l injection chromatograph of liquid of sample solution, records color
Spectrogram, measures, obtains final product.
Obviously, those skilled in the art can carry out the various changes and modification essence without deviating from the present invention to the present invention
God and scope.So, if these modifications of the present invention and modification belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprise these changes and modification.
Claims (3)
1. a kind of measure Cinnarizine capsule in Cinnarizine content method it is characterised in that with Cinnarizine reference substance for comparison, with
Methanol is mobile phase, using the content of Cinnarizine in high effective liquid chromatography for measuring Cinnarizine solid preparation；Wherein, specifically contain
Quantity measuring method is：
(1) chromatographic condition and its system suitability：Chromatographic column：C18 post 250 × 4.6mm；Mobile phase：Methanol；Flow velocity：1.2ml/
min；Detection wavelength：253nm；Sample size：10μl；40～50 DEG C of column temperature；System suitability：Number of theoretical plate is pressed Cinnarizine peak and is calculated
It is not less than 1000；
(2) preparation of reference substance solution：Take Cinnarizine reference substance appropriate, accurately weighed, plus methanol is configured to every 1ml and contains Cinnarizine
The solution of 1.3ug, obtains final product；
(3) preparation of need testing solution：Precision weighs Cinnarizine preparation or its content 13mg, weighed, puts in 100ml measuring bottle,
Plus methanol dissolves and is diluted to scale, shake up；Precision measures 1ml, puts in 100ml measuring bottle, plus methanol, to scale, shakes up, and obtains final product；
(4) algoscopy：Precision measures reference substance solution and each 10 μ l of need testing solution respectively, injects high performance liquid chromatograph, surveys
Determine Cinnarizine content.
2. a kind of method measuring Cinnarizine content in Cinnarizine capsule according to claim 1 is it is characterised in that described
Flow velocity is 1.0ml/min.
3. a kind of method measuring Cinnarizine content in Cinnarizine capsule according to claim 1 is it is characterised in that described
Column temperature is 45 DEG C.
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| CN108414636B (en) * | 2018-03-19 | 2021-02-19 | 河北科技大学 | Method for detecting cinnarizine related substances |
| CN110967421B (en) * | 2019-11-15 | 2022-04-12 | 正大青春宝药业有限公司 | Method for detecting related substances of flunarizine hydrochloride preparation |
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