CN103940923B - A kind of detection method of sumatriptan purity - Google Patents
A kind of detection method of sumatriptan purity Download PDFInfo
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- CN103940923B CN103940923B CN201410142236.9A CN201410142236A CN103940923B CN 103940923 B CN103940923 B CN 103940923B CN 201410142236 A CN201410142236 A CN 201410142236A CN 103940923 B CN103940923 B CN 103940923B
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- formic acid
- sumatriptan
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Abstract
The invention discloses a kind of detection method of sumatriptan purity, use HPLC-UV detection device to detect, adopt gradient elution mode to be separated, measure sumatriptan content by area normalization method, provide a kind of detection method of sumatriptan purity.
Description
Technical field
The invention belongs to the technical field of purity detecting, be specifically related to a kind of detection method of sumatriptan purity.
Background technology
Sumatriptan (Sumtriptan), chemistry 3-(2-dimethylamino) ethyl-N-methyl-1H-indoles-5-Methanesulfomide by name, it is the powerful 5-HT1B/1D receptor stimulating agent with high selectivity, entocranial artery can be made to shrink, blood redistributes, brain supply of blood flow is improved, thus extenuates obstinate headache outbreak rapidly, is the first aid medicine of antimigraine and cluster headache outbreak.Due to the advantage of the little and desirable selectivity anti-migraine activity of this medical instrument toxic side effect, its discovery is considered to a scientific breakthrough of antimigraine drug research, through development, sumatriptan has become first-line treatment medicine, has good clinical value.
Do not meet the method for detecting purity of sumatriptan characteristic at present, therefore, set up the mensuration of a kind of easy detection method accurately for sumatriptan purity, significant for sumatriptan quality monitoring.
Summary of the invention
The object of the invention is to the defect for above-mentioned existence and a kind of detection method of sumatriptan purity is provided, the purity of sumatriptan in sumatriptan finished product can be detected.
Technical scheme of the present invention is: a kind of detection method of sumatriptan purity, and the method adopts the highly effective liquid phase chromatographic system analysis in UV-detector to detect the purity of sumatriptan.
Adopt the concrete steps of the purity of the detection of the highly effective liquid phase chromatographic system analysis in UV-detector sumatriptan as follows:
(1) first get sumatriptan finished product sample acetonitrile to dissolve, then sample introduction injects UV-detector, analyzes under high performance liquid chromatography operating conditions;
(2) compose peak result according to step (1) high-efficient liquid phase color, carry out quantitatively to sumatriptan, quantivative approach adopts area normalization method.
High performance liquid chromatography operating conditions in described step (1): column temperature is 30 DEG C; Adopt gradient elution.
Chromatographic column in described UV-detector adopts octadecylsilane chemically bonded silica filler chromatographic column, is called for short ODS post or C again
18post.
The column length of described octadecylsilane chemically bonded silica filler chromatographic column is 25cm.
Stationary liquid film thickness in described octadecylsilane chemically bonded silica filler chromatographic column is 5 μm, and internal diameter is 4.6mm.
Determined wavelength in described UV-detector is 228nm, and mobile phase is the proportioning solution of 0.5g/L formic acid acetonitrile solution and 0.5g/L aqueous formic acid, flow velocity 1.0mL/min.
The sample size of described step (1) sample introduction is 20 μ L.
In described mobile phase, the ratio of formic acid acetonitrile solution and aqueous formic acid proportioning is 55:45 and 20:80.
Beneficial effect of the present invention is: the detection method of sumatriptan purity of the present invention, adopts gradient elution, and achieve being separated completely of sumatriptan and other impurity, all components all goes out peak within analysis time, and result is accurate; Usable floor area normalization method is quantitative, and quantivative approach is simple, reproducible.
Accompanying drawing explanation
Fig. 1 is sumatriptan purity testing chromatogram in the specific embodiment of the invention.
Wherein top is sumatriptan.
Embodiment
In order to understand the present invention better, describe technical scheme of the present invention in detail with specific embodiment below, but the present invention is not limited thereto.
Chromatographic column: C
18post (specification: 250mm × 4.6mm, 5 μm)
High performance liquid chromatography operating conditions: column temperature selects 30 DEG C, adopt gradient elution, wherein gradient is in table 1.
Table 1: proportion of mobile phase
Prepared by sample solution: take 0.0025g sample in 10mL volumetric flask, with acetonitrile dissolved dilution to scale, shake up, excessively sample introduction analysis after 0.45 μm of organic filter membrane;
Sample size: 20 μ L;
Carry out quantitatively, according to w with area normalization method to sumatriptan
i=(A
i/ ∑ A
i) × 100 calculate sumatriptan purity in sample, wherein: w
ithe percentage composition of each component in-sample, %; A
ithe peak area of each component in-sample.
Standard deviation (method precision) is tested: get the sumatriptan that 3 kinds of different manufacturers are produced, and numbering is respectively 1
#, 2
#, 3
#, measure as stated above, according to the peak area of component each in chromatogram, according to the percentage composition of sumatriptan in formulae discovery sample.Often kind of sample parallel measures 5 times, and result of calculation is in table 2.
Table 2: sample determination and precision result (n=5)
Method accuracy test: take content be >=99.9% sumatriptan standard items measure as stated above, according to the peak area of component each in chromatogram, according to the percentage composition of sumatriptan in formulae discovery sample, replicate determination 5 times, result of calculation is in table 3.
Table 3: method accuracy test result
Gradient Comparability test: adopt different proportion mobile phase isocratic elution to measure 2 respectively
#sample, usable floor area normalization method, according to the percentage composition of sumatriptan in formulae discovery sample, measurement result is in table 4, and the degree of separation of comprehensive main peak and other impurities component, the factor such as peak shape and test duration, adopt linear gradient elution method in the present invention.
Table 4: isocratic elution measurement result
Quantivative approach Comparability test: adopt single-point external standard method to measure 1 respectively
#, 2
#, 3
#sample, under identical chromatographic condition, often kind of sample parallel measures 5 times, and measurement result is in table 5.
Table 5: single-point external standard method sample determination and precision result (n=5)
The advantage of reference area normalization method and single-point external standard determination data: single-point poor repeatability, the impact of integral area is very large, and because computation process needs to use quality, and it is less to weigh quality, or needs dilution, and therefore, the impact that weighing or dilution are introduced is larger.And area normalization method does not weigh or dilute the impact of introducing, quantivative approach is simple, reproducible.
Experiment proves, the detection method of a kind of sumatriptan purity of the present invention, and result is accurate, and method is simple, reproducible.
Claims (4)
1. a detection method for sumatriptan purity, is characterized in that, the method adopts the highly effective liquid phase chromatographic system analysis of band UV-detector to detect the purity of sumatriptan; Adopt the concrete steps of the purity of the highly effective liquid phase chromatographic system analysis detection sumatriptan of band UV-detector as follows: (1) is first got sumatriptan finished product sample acetonitrile and dissolved, then sample introduction injects highly effective liquid phase chromatographic system, analyzes under high performance liquid chromatography operating conditions; (2) compose peak result according to step (1) high-efficient liquid phase color, carry out quantitatively to sumatriptan, quantivative approach adopts area normalization method; High performance liquid chromatography operating conditions in described step (1): column temperature is 30 DEG C; Adopt gradient elution; Determined wavelength in described UV-detector is 228nm, and mobile phase is the proportioning solution of 0.5g/L formic acid acetonitrile solution and 0.5g/L aqueous formic acid, flow velocity 1.0mL/min; In described mobile phase, formic acid acetonitrile solution and the ratio of aqueous formic acid in gradient elution process are: initial flow matched is 0.5g/L formic acid acetonitrile solution: 0.5g/L aqueous formic acid=55:45, keep 18min; In 18 min ~ 37min, proportion of mobile phase is by 0.5g/L formic acid acetonitrile solution: 0.5g/L aqueous formic acid=55:45 is changed to 0.5g/L formic acid acetonitrile solution: 0.5g/L aqueous formic acid=20:80; In 37min ~ 38min, proportion of mobile phase is by 0.5g/L formic acid acetonitrile solution: 0.5g/L aqueous formic acid=20:80 is changed to 0.5g/L formic acid acetonitrile solution: 0.5g/L aqueous formic acid=55:45, finally by proportion of mobile phase 0.5g/L formic acid acetonitrile solution: 0.5g/L aqueous formic acid=55:45 keeps 4min; Chromatographic column in described highly effective liquid phase chromatographic system adopts octadecylsilane chemically bonded silica filler chromatographic column.
2. the detection method of sumatriptan purity according to claim 1, it is characterized in that, the column length of described octadecylsilane chemically bonded silica filler chromatographic column is 25cm.
3. the detection method of sumatriptan purity according to claim 2, it is characterized in that, the Stationary liquid film thickness in described octadecylsilane chemically bonded silica filler chromatographic column is 5 μm, and internal diameter is 4.6mm.
4. the detection method of sumatriptan purity according to claim 1, it is characterized in that, the sample size of described step (1) sample introduction is 20 μ L.
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| CN103940923B true CN103940923B (en) | 2015-09-23 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212027A (en) * | 2011-05-04 | 2011-10-12 | 苏州莱克施德药业有限公司 | Preparation method for sumatriptan |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005123043A2 (en) * | 2004-06-10 | 2005-12-29 | Duramed Pharmaceuticals, Inc. | Formulations of sumatriptan for absorption across biological membranes, and methods of making and using the same |
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2014
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212027A (en) * | 2011-05-04 | 2011-10-12 | 苏州莱克施德药业有限公司 | Preparation method for sumatriptan |
Non-Patent Citations (4)
| Title |
|---|
| Determination of degradation products of sumatriptan succinate using LC-MS and LC-MS-MS;Xiaohui Xu et al.;《Journal of Pharmaceutical and Biomedical Analysis》;20011031;第26卷(第3期);367-377 * |
| Impurities profiling Method and degradation studies for Sumatriptan Succinate in Sumatriptan Succinate and Naproxen Sodium Tablets;Palavai Sripal reddy et al.;《Journal of Chemical and Pharmaceutical Research》;20121231;第4卷(第6期);3263-3274 * |
| 舒马曲坦的合成;王绍杰 等;《中国药物化学杂志》;20081231;第18卷(第6期);442-444 * |
| 舒马曲坦胶囊的制备与质量控制;张敬如 等;《中国药业》;20121105;第21卷(第21期);32-34 * |
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