CN106855542A - Method of the high performance liquid chromatography detection metadoxine about material - Google Patents
Method of the high performance liquid chromatography detection metadoxine about material Download PDFInfo
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Abstract
The invention belongs to Pharmaceutical Analysis technical field, specifically, it is related to a kind of high performance liquid chromatography detection metadoxine about the method for material, metadoxine need testing solution and reference substance solution are detected respectively using high performance liquid chromatography, the chromatogram of the two is recorded and is obtained the peak area of vitamin B6 alkali in the metadoxine need testing solution and the main peak area of the reference substance solution and quantitative analysis is carried out to the relevant material of metadoxine with external standard method；The reference substance solution is metadoxine sterling solution.The method separating degree is high, principal component retention time moderate i.e. analysis time is short, low cost.
Description
Technical field
The invention belongs to Pharmaceutical Analysis technical field, in particular to a kind of high performance liquid chromatography detection metadoxine
About the method for material.
Background technology
Metadoxine, chemical entitled pyridoxol L-2 pyrrolidone-5-carboxylic acid salt is shown under its chemical constitution such as formula；
Metadoxine is developed by Italian Laboratori Baldacci SPA companies, and in September, 1985 is in Italy
Listing, trade name Metadoxil；Metadoxine can reduce ethanol in blood, and internal ethanol mainly turns through alcohol dehydrogenase (ADH)
Acetaldehyde is turned to, acetaldehyde is converted into through microsomal ethanol oxidase on a small quantity, acetaldehyde is converted into acetic acid through acetaldehyde dehydrogenase (ALDH) again,
Again CO is finally oxidized to through tricarboxylic acid cycle2And H2O.The vigor of intrahepatic metabolism enzyme is depended primarily on because of the accretion rate of ethanol, therefore
Ying Yuqi can prevent the inactivation of ADH relevant, and internal ADH can be made to maintain normal level, also there are some researches show metadoxine can add
, through RE, its indication is AML for fast ethanol and its metabolite acetaldehyde and ketoboidies.Patients with alcoholic liver disease group
Body is huge, and has growth trend, and metadoxine can improve due to caused by long-term alcohol as treatment alcoholic liver medicine
Hepatic disorder.As metadoxine medicine is widely used, crowd's concern is benefited from by vast as its quality of medicine, and it is existing
Metadoxine quality research is less, therefore, the quality research of metadoxine is significant to its quality control.
At present, detected using Luna C18 (2), Agilen Zorbax SB-C18 chromatographic columns in the prior art it is beautiful he
More pungent main component and relevant material, when being detected using this kind of chromatographic column, sample retention time is oversize, and separating degree is small etc.
Shortcoming；Causing relevant material if attempting shortening retention time can not efficiently separate with main component pyroglutamic acid；Therefore find
A kind of separating degree is high, principal component retention time moderate i.e. analysis time is short, low cost detection method is necessary.
In view of this, it is special to propose the present invention.
The content of the invention
It is an object of the invention to provide a kind of high performance liquid chromatography detection metadoxine about material method, with solve
Above mentioned problem.
In order to realize above-mentioned purpose of the invention, spy uses following technical scheme：
A kind of high performance liquid chromatography detection metadoxine about material method, including：
Metadoxine need testing solution and reference substance solution are detected respectively using high performance liquid chromatography, record two
The chromatogram of person simultaneously obtains the peak area and the reference substance solution of vitamin B6 alkali in the metadoxine need testing solution
Main peak area simultaneously carries out quantitative analysis with external standard method to the relevant material of metadoxine；
The reference substance solution is metadoxine sterling solution.
The present invention carries out quantitative analysis using external standard method, no matter the whether whole appearances of all components in sample, can be right
Appearance component does quantitative analysis.For quantitatively reference substance, external standard method is method the most accurate, because being that homogeneity component is carried out
Compare.
Preferably, high performance liquid chromatography detection metadoxine as described above about material method, the metadoxine
The concentration of need testing solution be 0.2mg/ml~1mg/ml, more preferably 0.3mg/ml~0.6mg/ml, it is also an option that
0.4mg/ml。
Preferably, high performance liquid chromatography detection metadoxine as described above is about the method for material, and the reference substance is molten
The concentration of liquid is 0.04 μ g/ml~10 μ g/ml, more preferably 0.08 μ g/ml~8 μ g/ml, more preferably 0.5 μ g/ml~6 μ g/
Ml, it is also an option that 1 μ g/ml, 2 μ g/ml or 4 μ g/ml etc..
Preferably, high performance liquid chromatography detection metadoxine as described above is carrying out efficient liquid about the method for material
When phase chromatogram is detected, the fixing phase of chromatographic column used is full multi-hole blangel particulate bonding C8 functional groups, and mobile phase is acetonitrile-water
Mixed solution.
Preferably, high performance liquid chromatography detection metadoxine as described above about material method, the chromatographic column
Specification is：
Internal diameter is 4.2~5.0mm, and length is 200~300mm, and packing material size is 2~8 μm.More preferably internal diameter is
4.6mm, length is 250mm, and packing material size is 5 μm.
Preferably, about the method for material, the chromatographic column is high performance liquid chromatography detection metadoxine as described above
Inertsil C8-4。
Preferably, high performance liquid chromatography detection metadoxine as described above about material method, the acetonitrile-water
Acetonitrile and the volume ratio of water are 1 in mixed solution：99~10：90, and it is 1.0~3.0 to adjust flowing phase pH value with phosphoric acid；It is preferred that
The acetonitrile-water mixed solution in the volume ratio of acetonitrile and water be 1：99~5：90, and adjust flowing phase pH value with phosphoric acid
It is 1.5~2.5；
Preferably, high performance liquid chromatography detection metadoxine as described above about material method, the mobile phase
Flow velocity is 0.5ml/min~1.5ml/min；It is furthermore preferred that flow velocity is 0.8ml/min-1.2ml/min, it is also an option that
0.6ml/min, 1.0ml/min etc..
The size of flow velocity directly influences the consumption problem of mobile phase, but from for economic angle, it should setting is smaller
Flow velocity；Because the filling of pillar and instrument relation in itself can not set excessive flow velocity.
Preferably, high performance liquid chromatography detection metadoxine as described above about material method, the chromatographic column
Column temperature is 10 DEG C~40 DEG C, more preferably 25 DEG C~35 DEG C.
Retention time influence when column temperature is on wash-out is larger, and with the rising of column temperature, retention time can typically decline.
Preferably, high performance liquid chromatography detection metadoxine as described above is carrying out efficient liquid about the method for material
When phase chromatogram is detected, Detection wavelength is 200nm~300nm, more preferably 200nm~210nm, it is also an option that 205nm；Efficiently
Liquid chromatogram single injected sampling amount is 3 μ l~7 μ l, more preferably 5 μ l.
Compared with prior art, beneficial effects of the present invention are：
1), compared with prior art, the inventive method have separating degree higher, in metadoxine contained vitamin B6 with
Pyroglutamic acid main component separating degree is more than 7.0, and chromatogram main peak theoretical tray is more than 10000, and peak shape is sharp, symmetrical.
2), the present invention is second eyeball-water (1% in mobile phase：99%, when 2.0) phosphoric acid tune pH value is, you can he is more to ensure U.S.
The pungent main separating degree of principal component can make principal component be more than 6.0 with the separating degree of major impurity more than 7.0, again, and when retaining
Between within 10min, be provided simultaneously with the advantages of separating degree is high, analysis time is short.
3), the present invention using flowing phased soln metadoxine, its solubility is higher, dissolution velocity faster, can be effective
Avoid separating out solid and causing the blocking of chromatographic column and chromatographic system in detection process so that testing result accurately and reliably, its
Operation is also easier.
Brief description of the drawings
In order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art, below will be to specific
The accompanying drawing to be used needed for implementation method or description of the prior art is briefly described, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 detects chromatogram for the liquid phase under the conditions of embodiment 1 to metadoxine；
Fig. 2 detects chromatogram for the liquid phase under the conditions of embodiment 2 to metadoxine；
Fig. 3 detects chromatogram for the liquid phase under the conditions of embodiment 3 to metadoxine；
Fig. 4 detects chromatogram for the liquid phase under the conditions of embodiment 4 to metadoxine；
Fig. 5 is the linear relationship of detection method.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, are
The conventional products for obtaining can be bought by city.
The test sample that is used in the specific embodiment of the invention, reference substance, equipment are known product, and wherein reference substance exists
National Institute for Food and Drugs Control buys
High performance liquid chromatograph：Angilent1260 high performance liquid chromatographs, DAD detectors
The method of measure metadoxine content of the invention is made in detailed below with specific embodiment with reference to Figure of description
Explanation.
Embodiment 1
Metadoxine high-efficiency liquid chromatography method for detecting：
(1) need testing solution is prepared：Precision weighs metadoxine 5mg, in putting 25ml measuring bottles, plus flowing phased soln and dilutes
To scale, shake up, as need testing solution.
Prepare reference substance solution：The relevant substance A 5mg of metadoxine is taken, is placed in 25ml measuring bottles, plus flowing phased soln is simultaneously
Scale is diluted to, is shaken up, as reference substance storing solution；Precision is measured in right amount, and quantitative dilution contains 0.2 μ g's in being made every 1ml
Solution, as reference substance solution
Preparation system employment and suitability test (E ＆ ST) solution：Metadoxine 5mg is taken, is placed in 25ml measuring bottles, plus flowing phased soln and dilute
Release to scale, shake up, obtain metadoxine solution；Take reference substance storing solution 0.25ml, be placed in 25ml measuring bottles, with it is above-mentioned it is beautiful he
More pungent solution is diluted to scale, shakes up, used as system suitability solution；
(2) testing conditions of high performance liquid chromatography are：
Chromatographic column：Inertsil C8-4(4.6mm×260mm 5μm)
Mobile phase：Acetonitrile-water (1%：99%) it is 2.0 that, phosphoric acid adjusts pH value
Flow velocity：0.8ml/min
Detection wavelength：205nm
Column temperature：25℃
According to above-mentioned testing conditions, the μ l of system suitability solution 5 injection liquid chromatographs are taken, record chromatogram, taken
The μ l of reference substance 5 inject liquid chromatograph, adjust detection sensitivity, make the 10% of principal component chromatographic peak peak height about full scale；Essence
It is close to measure need testing solution and each 5 μ l of reference substance solution, liquid chromatograph is injected separately into, chromatogram is recorded, by external standard method with peak
The content of areal calculation experimental cultivar metadoxine impurity is about 0.02%.
Computing formula：
The relevant material of metadoxine
In formula：
ASample：The peak area of vitamin B6 alkali in confession under directions test sample solution；
AIt is right：Refer to reference substance solution main peak area
CSample：Concentration (the unit of confession under directions test sample solution：mg/ml)
CIt is right：Refer to the concentration (unit of reference substance solution：μg/ml)
Metadoxine main component vitamin B6, pyroglutamic acid, the separating effect about substance A under the conditions of the embodiment 1 of table 1
Note：The result of calculation of 2#, 3# separating degree is related with 1#
Result shows that detection method metadoxine principal component vitamin B6 is 7.31 with pyroglutamic acid separating degree,
Vitamin B6 alkali and relevant substance A separating degree 6.53, theoretical tray is all higher than 51000, far above prior art separating degree and
Theoretical cam curve, effectively avoids the accuracy of the interference effect testing result of each component；Meanwhile, detection method is beautiful
In Ta Duoxin principal component with the retention time about substance A within 10min, with analysis time is short, low cost and other advantages.
Embodiment 2
Mobile phase is changed to acetonitrile-water (5% in testing conditions：95%) it is 2.0, other steps and implementation that, phosphoric acid adjusts pH value
Condition is with embodiment 1.
According to above-mentioned testing conditions, the μ l of system suitability solution 5 injection liquid chromatographs are taken, record chromatogram, taken
The μ l of reference substance 5 inject liquid chromatograph, adjust detection sensitivity, make the 10% of principal component chromatographic peak peak height about full scale；Essence
It is close to measure need testing solution and each 5 μ l of reference substance solution, liquid chromatograph is injected separately into, chromatogram is recorded, by external standard method with peak
The content of areal calculation experimental cultivar metadoxine impurity is about 0.02%.
Metadoxine main component vitamin B6, pyroglutamic acid, the separation effect about substance A under the conditions of table 2, embodiment 2
Really
Note：The result of calculation of 2#, 3# separating degree is related with 1#
Result shows that detection method metadoxine principal component vitamin B6 is 3.27 with pyroglutamic acid separating degree,
Vitamin B6 alkali and relevant substance A separating degree 8.43, theoretical tray is all higher than 54000, far above prior art separating degree and
Theoretical cam curve, effectively avoids the accuracy of the interference effect testing result of each component；Meanwhile, detection method is beautiful
In Ta Duoxin principal component with the retention time about substance A within 10min, with analysis time is short, low cost and other advantages.
Embodiment 3
Flow velocity is changed into 1.0ml/min in testing conditions, and other steps and implementation condition are with embodiment 1.
According to above-mentioned testing conditions, the μ l of system suitability solution 5 injection liquid chromatographs are taken, record chromatogram, taken
The μ l of reference substance 5 inject liquid chromatograph, adjust detection sensitivity, make the 10% of principal component chromatographic peak peak height about full scale；Essence
It is close to measure need testing solution and each 5 μ l of reference substance solution, liquid chromatograph is injected separately into, chromatogram is recorded, by external standard method with peak
The content of areal calculation experimental cultivar metadoxine impurity is about 0.02%.
Metadoxine main component vitamin B6, pyroglutamic acid, the separation effect about substance A under the conditions of table 3, embodiment 3
Really
Note：The result of calculation of 2#, 3# separating degree is related with 1#
Result shows that detection method metadoxine principal component vitamin B6 is 6.36 with pyroglutamic acid separating degree,
Vitamin B6 alkali and relevant substance A separating degree 8.08, theoretical tray is all higher than 44000, far above prior art separating degree and
Theoretical cam curve, effectively avoids the accuracy of the interference effect testing result of each component；Meanwhile, detection method is beautiful
In Ta Duoxin principal component with the retention time about substance A within 10min, with analysis time is short, low cost and other advantages.
Embodiment 4
Column temperature is changed into 35 DEG C in testing conditions, and other steps and implementation condition are with embodiment 1.
According to above-mentioned testing conditions, the μ l of system suitability solution 5 injection liquid chromatographs are taken, record chromatogram, taken
The μ l of reference substance 5 inject liquid chromatograph, adjust detection sensitivity, make the 10% of principal component chromatographic peak peak height about full scale；Essence
It is close to measure need testing solution and each 5 μ l of reference substance solution, liquid chromatograph is injected separately into, chromatogram is recorded, by external standard method with peak
The content of areal calculation experimental cultivar metadoxine impurity is about 0.02%.
Metadoxine main component vitamin B6, pyroglutamic acid, the separation effect about substance A under the conditions of table 4, embodiment 4
Really
Note：The result of calculation of 2#, 3# separating degree is related with 1#
Result shows that detection method metadoxine principal component vitamin B6 is 7.48 with pyroglutamic acid separating degree,
Vitamin B6 alkali and relevant substance A separating degree 6.86, theoretical tray is all higher than 55000, far above prior art separating degree and
Theoretical cam curve, effectively avoids the accuracy of the interference effect testing result of each component；Meanwhile, detection method is beautiful
In Ta Duoxin principal component with the retention time about substance A within 10min, with analysis time is short, low cost and other advantages.
Test example 1, linear relationship
(1) it is appropriate that need testing solution is taken respectively, plus mobile phase is made the series confession that concentration is 0.05 μ g/ml~1.5 μ g/ml
Test sample solution；
(2) above-mentioned need testing solution is detected according to the testing conditions of embodiment 1, records chromatogram, he is more with U.S.
The concentration of pungent middle vitamin B6 alkali carries out linear regression, linear equation to corresponding peak area：Y=16.20x+0.280 is related
Coefficients R2=0.999, as shown in Figure 5.
Test result indicate that, under conditions of detection method, concentration and peak area line of the metadoxine about substance A
Sexual intercourse is good.
Test example 2, test limit is tested
The a height of 222uv of reference substance solution main peak of least concentration in linear relationship experiment, baseline noise is about 5uv, noise
Than being about 44:1, according to test limit requirement, (signal to noise ratio should be 3:1), be respectively configured 0.02,0.002,0.0002 μ g/ml it is beautiful he
It is more pungent to photo solution, according to the testing conditions of embodiment 1, sample introduction is determined, and records chromatogram.
In metadoxine the minimum detectable activity of vitamin B6 be 0.02ng, pyroglutamic acid minimum detectable activity be 0.2ng, experiment
Result shows, detection method of the invention is low to the main component vitamin B6 of metadoxine, pyroglutamic acid test limit.
Test example 3, precision test
By preparing potential known impurities, the pin of continuous sample introduction 6 records chromatogram, investigates separating degree and peak area, it is desirable to
The RSD for determining 6 results cannot be greater than 5.0%, and carrying out substantive approach has good sample introduction precision, and determines each known simultaneously
The correction factor of impurityAnd relative retention time.
MT-1, MT-2, MT-3, MT-4 each 5mg of impurity reference substance are weighed respectively, are placed in 25ml measuring bottles, plus flowing mixes
Scale is solved and be diluted to, is shaken up；Take respectively during 1ml puts 100ml measuring bottles, plus mobile phase is diluted to scale, shakes up molten as testing
Liquid
According to the testing conditions of embodiment 1, the μ l of test solution 5 are taken, inject liquid chromatograph, METHOD FOR CONTINUOUS DETERMINATION 6 times, record
Chromatogram.Testing result is shown in Table 6.
Table 6, each impurity reference substance retention time precision investigate result
| Component | 1 | 2 | 3 | 4 | 5 | 6 | Averagely | RSD% |
| MT-1 | 5.659 | 5.675 | 5.657 | 5.658 | 5.657 | 5.657 | 5.6605 | 0.08 |
| MT-2 | 6.163 | 6.190 | 6.170 | 6.165 | 6.166 | 6.161 | 6.1691 | 0.12 |
| MT-3 | 7.101 | 7.133 | 7.110 | 7.109 | 7.104 | 7.102 | 7.1098 | 0.11 |
| MT-4 | 10.317 | 10.361 | 10.338 | 10.326 | 10.317 | 10.314 | 10.3288 | 0.13 |
According to table 6 as can be seen that after reference substance solution continuous sample introduction 6 times, the equal ＜ 2.0% of RSD of each impurity retention time,
Sample introduction precision is good.
The specificity of test example 4, method
The discriminating at the specificity study tour peak of method and selectivity, it is desirable to：Difference sample introduction blank solution and all positioning
Solution cannot be less than 1.5 determining all potential impurity, main peak with the separating degree between adjacent chromatographic peak.
Known impurities MT-1, MT-2, MT-3, MT-4 are configured to the positioning solution of concentration about 0.2mg/ml respectively, will
Above-mentioned impurity positioning solution is respectively taken during 1ml puts same 10ml measuring bottles, plus mobile phase is diluted to scale, shakes up that to obtain impurity mixing molten
Liquid.It is another to take metadoxine 5mg to 25ml volumetric flasks, and impurity mixed solution 0.25ml is taken in this measuring bottle, plus mobile phase is dilute
Release to scale, shake up as mixed solution
According to the testing conditions of embodiment 1, by blank (mobile phase), each positioning solution and each 5 μ l injections of mixed solution
Liquid chromatograph, records chromatogram.Testing result is shown in Table 5.
Table 5, mixed solution separating degree test result
| Compound numbers | Retention time (min) | Separating degree | Theoretical cam curve | The purity factor |
| Blank | 2.035 | / | / | / |
| MT-1 | 5.645 | / | 14092 | 999.862 |
| MT-2 | 6.358 | 3.79 | 18863 | 999.452 |
| MT-3 | 7.388 | 5.23 | 20211 | 999.354 |
| MT-4 | 10.855 | 13.55 | 20547 | 999.615 |
According to table 5 as can be seen that blank does not disturb metadoxine about the detection of material, its defects inspecting is not disturbed yet.
Each impurity can be separated efficiently in metadoxine, and separating degree is all higher than 2.0, and peak shape is good, and peak purity is good, theoretical tray
Number is more than 3000, and tailing factor is less than 1.5, meets standard.
Although illustrate and describing the present invention with specific embodiment, but will be appreciated that without departing substantially from of the invention
Many other changes and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. method of a kind of high performance liquid chromatography detection metadoxine about material, it is characterised in that including：
Metadoxine need testing solution and reference substance solution are detected respectively using high performance liquid chromatography, the two is recorded
Chromatogram simultaneously obtains the peak area of vitamin B6 alkali in the metadoxine need testing solution and the main peak of the reference substance solution
Area simultaneously carries out quantitative analysis with external standard method to the relevant material of metadoxine；
The reference substance solution is metadoxine sterling solution.
2. method of the high performance liquid chromatography detection metadoxine according to claim 1 about material, it is characterised in that institute
The concentration for stating metadoxine need testing solution is 0.2~1mg/ml.
3. method of the high performance liquid chromatography detection metadoxine according to claim 1 about material, it is characterised in that institute
It is 0.04 μ g/ml~10 μ g/ml to state the concentration of reference substance solution.
4. method of the high performance liquid chromatography detection metadoxine according to claim 1 about material, it is characterised in that
When carrying out high performance liquid chromatography detection, the fixing phase of chromatographic column used is full multi-hole blangel particulate bonding C8 functional groups, mobile phase
It is the mixed solution of acetonitrile-water.
5. method of the high performance liquid chromatography detection metadoxine according to claim 4 about material, it is characterised in that institute
The specification for stating chromatographic column is：
Internal diameter is 4.2~5.0mm, and length is 200~300mm, and packing material size is 2~8 μm.
6. method of the high performance liquid chromatography detection metadoxine according to claim 4 about material, it is characterised in that institute
Chromatographic column is stated for Inertsil C8-4.
7. method of the high performance liquid chromatography detection metadoxine according to claim 4 about material, it is characterised in that institute
The volume ratio for stating acetonitrile and water in the mixed solution of acetonitrile-water is 1：99~10：90, and be with phosphoric acid regulation flowing phase pH value
1.0~3.0.
8. method of the high performance liquid chromatography detection metadoxine according to claim 4 about material, it is characterised in that institute
The flow velocity for stating mobile phase is 0.5ml/min~1.5ml/min.
9. method of the high performance liquid chromatography detection metadoxine according to claim 4 about material, it is characterised in that institute
The column temperature for stating chromatographic column is 10 DEG C~40 DEG C.
10. method of the high performance liquid chromatography detection metadoxine according to claim 1 about material, it is characterised in that
When high performance liquid chromatography detection is carried out, Detection wavelength is 200nm~300nm；High performance liquid chromatography single injected sampling amount be 3 μ l~
7μl。
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| CN107991415A (en) * | 2018-01-17 | 2018-05-04 | 南京医科大学康达学院 | With the method for pyroglutamic acid and methionine sulfoxide impurity in liquid chromatography at the same time separation determination Amino Acid Compound Injection 18AA |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107991415A (en) * | 2018-01-17 | 2018-05-04 | 南京医科大学康达学院 | With the method for pyroglutamic acid and methionine sulfoxide impurity in liquid chromatography at the same time separation determination Amino Acid Compound Injection 18AA |
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