CN108459106A - A kind of method of homopiperazine content in measurement Fasudic hydrochloride - Google Patents
A kind of method of homopiperazine content in measurement Fasudic hydrochloride Download PDFInfo
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- CN108459106A CN108459106A CN201810388106.1A CN201810388106A CN108459106A CN 108459106 A CN108459106 A CN 108459106A CN 201810388106 A CN201810388106 A CN 201810388106A CN 108459106 A CN108459106 A CN 108459106A
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Abstract
The present invention provides a kind of method measuring homopiperazine content in Fasudic hydrochloride, and in particular to drug measurement techniques field includes the following steps：S1, homopiperazine reference substance is taken, using 5% acetonitrile solution as solvent, prepares homopiperazine reference substance solution, take Fasudic hydrochloride, using 5% acetonitrile solution as solvent, prepare test solution；Two parts of S2, parallel preparation homopiperazine reference substance solutions are detected through UPLC MS methods, obtain the peak area of homopiperazine in reference substance solution respectively, are calculated the ratio of the concentration of peak area and reference substance solution, are obtained the response factor of homopiperazine；S3, it takes test solution to be detected through UPLC MS methods, obtains the peak area of test solution, the content of homopiperazine in test solution is calculated with response factor.The present invention has detection time short, and accuracy is good, and precision is high, reproducible advantage.
Description
Technical field
The invention belongs to drug measurement techniques fields, and in particular to a kind of to measure homopiperazine content in Fasudic hydrochloride
Method.
Background technology
Fasudic hydrochloride is a kind of myosin light chain phosphorylase, RHO kinase inhibitors and novel fine cellular calcium from
Sub- anticaking agent, the medicine can improve brain tissue microcirculation, and cerebral angiospasm is effectively relieved, and protect ischemic tissue of brain, promote nerve again
It is raw, it is a kind of newtype drug with extensive pharmacological action, homopiperazine is the intermediate in Fasudic hydrochloride building-up process, by
In homopiperazine without UV absorption, polarity is big, can not effectively be detected using high performance liquid chromatography, has document report and uses
The content of homopiperazine in liquid chromatography, ultraviolet spectrophotometry, ion-chromatographic determination Fasudic hydrochloride, but existing inspection
Survey method measurement structural fidelity is low, cumbersome.
Therefore, it is simple to be badly in need of a kind of method, splitter effect is high, and accuracy is high, simple and easy to do, can be used for Fasudic hydrochloride
The method for measuring homopiperazine content in Fasudic hydrochloride of quality control in production process.
Invention content
In order to solve the problem that the accuracy of homopiperazine content assaying method is low, cumbersome in existing Fasudic hydrochloride,
The object of the present invention is to provide a kind of methods of homopiperazine content in measurement Fasudic hydrochloride, have detection time short, accurately
It spends, precision is high, reproducible advantage.
The present invention provides the following technical solutions：
The method of homopiperazine content, includes the following steps in a kind of measurement Fasudic hydrochloride：
S1, homopiperazine reference substance is taken, using 5% acetonitrile solution as solvent, prepares homopiperazine reference substance solution, take hydrochloric acid method
The ground that relaxes prepares test solution using 5% acetonitrile solution as solvent；
Two parts of S2, parallel preparation homopiperazine reference substance solutions are detected through UPLC-MS methods, are obtained in reference substance solution respectively
The peak area of homopiperazine calculates the ratio of the concentration of peak area and reference substance solution, obtains the response factor of homopiperazine；
S3, it takes test solution to be detected through UPLC-MS methods, obtains the peak area of test solution, calculated with response factor
The content of homopiperazine in test solution.
Preferably, the chromatographic condition of UPLC-MS methods is in the S2 steps and the S3 steps：Using CSH C18 chromatographies
Column (2.1 × 100mm, 1.7 μm), column temperature are 35 DEG C；5 μ L of sample size；Detector is mass detector, ion source ESI, just from
Subpattern, ion 101；Using 0.1% formic acid as mobile phase A, acetonitrile is Mobile phase B, flow velocity 0.2mL/min；Gradient elution
Program is：The percentage by volume of 0~1min, Mobile phase B are 5%；1~5min, the percentage by volume of Mobile phase B by 5% to
90%；5~5.1min, the percentage by volume of Mobile phase B is by 90% to 5%；The percentage by volume of 5.1~7min, Mobile phase B is
5%.
Gradient elution program
| T/min | 0.1% formic acid | Acetonitrile |
| 0 | 95 | 5 |
| 1 | 95 | 5 |
| 5 | 10 | 90 |
| 5.1 | 95 | 5 |
| 7 | 95 | 5 |
The beneficial effects of the invention are as follows：
1, the UPLC-MS methods that the present invention uses measure homopiperazine content, since compound homopiperazine is that hydrochloric acid method relaxes ground
Your catabolite, the accuracy in the methodology validation of gas chromatography are unable to reach testing requirements；And homopiperazine is without ultraviolet
Response absorbs, therefore selects to use UPLC-MS methods, homopiperazine can be accurately positioned, specificity is strong, high sensitivity.
2, using UPLC-MS methods, chromatographic time is short, not only saves detection time and greatly reduces organic solvent
It uses, the harm to environment is reduced while improving efficiency.
3, under the conditions of UPLC-MS provided by the invention, by the homopiperazine content in external standard method test solution,
It is easy to operate, and methodology validation has been carried out, the experimental results showed that the detection method specificity of this method is strong, accuracy is good,
Precision is high, reproducible, meets the technology requirement of the quality standard research of drug.
Description of the drawings
Attached drawing is used to provide further understanding of the present invention, and a part for constitution instruction, the reality with the present invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings：
Fig. 1 is 1 reference substance solution of embodiment and test solution chromatogram；
Fig. 2 is the IPTG canonical plottings that 2 range of linearity of embodiment is investigated；
Fig. 3 is the specificity collection of illustrative plates of 5 specificity of embodiment experiment.
Specific implementation mode
Embodiment 1
The method of homopiperazine content, includes the following steps in a kind of measurement Fasudic hydrochloride：
S1, homopiperazine reference substance is taken, using 5% acetonitrile solution as solvent, prepares the homopiperazine reference substance solution of 3 μ g/mL,
Fasudic hydrochloride is taken, using 5% acetonitrile solution as solvent, prepares the test solution of 1.5mg/mL；
Two parts of S2, parallel preparation homopiperazine reference substance solutions are detected through UPLC-MS methods, are obtained in reference substance solution respectively
The peak area of homopiperazine calculates the ratio of the concentration of peak area and reference substance solution, obtains the response factor of homopiperazine；
S3, it takes test solution to be detected through UPLC-MS methods, obtains the peak area of test solution, calculated with response factor
The content of homopiperazine in test solution.
Specifically, the chromatographic condition of UPLC-MS methods is in S2 steps and S3 steps：Using CSH C18 chromatographic columns (2.1 ×
100mm, 1.7 μm), column temperature is 35 DEG C；5 μ L of sample size；Detector is mass detector, ion source ESI, positive ion mode,
Ion is 101；Using 0.1% formic acid as mobile phase A, acetonitrile is Mobile phase B, flow velocity 0.2mL/min；Gradient elution program is：0
The percentage by volume of~1min, Mobile phase B are 5%；1~5min, the percentage by volume of Mobile phase B is by 5% to 90%；5~
5.1min, the percentage by volume of Mobile phase B is by 90% to 5%；The percentage by volume of 5.1~7min, Mobile phase B are 5%.
The test data of gradient elution program is as shown in table 1.
1 gradient elution program of table
| T/min | 0.1% formic acid | Acetonitrile |
| 0 | 95 | 5 |
| 1 | 95 | 5 |
| 5 | 10 | 90 |
| 5.1 | 95 | 5 |
| 7 | 95 | 5 |
Using the gradient elution program provided in embodiment 1, UPLC- is carried out to reference substance solution and test solution respectively
MS is analyzed, and for gained chromatogram as shown in Figure 1, figure label 2 is reference substance solution, label 3 is test solution, shows homopiperazine
Retention time be 0.896min.
Embodiment 2
The range of linearity for the assay method that embodiment 1 provides is investigated
It takes in 41.87mg homopiperazines to 25mL volumetric flasks, after adding 5% acetonitrile to dissolve, is settled to scale, shakes up, as height
Piperazine stock solution A；Precision pipettes 1.0mL homopiperazine stock solution A to 10mL volumetric flasks, adds 5% dilution in acetonitrile and constant volume, shakes up,
As homopiperazine stock solution B；Precision pipettes 0.4mL homopiperazine stock solution B to 10mL volumetric flasks, adds 5% dilution in acetonitrile and constant volume,
It shakes up, as homopiperazine stock solution C；0.3350 μ g/mL, 0.6699 μ g/mL, 1.3398 μ g/mL, 2.0098 μ g/mL are prepared,
2.6797 μ g/mL, 3.3496 μ g/mL, 5.0244 μ g/mL and 6.6992 μ g/mL linear solvents, are respectively labeled as LOQ, and 20%,
40%, 60%, 80%, 100%, 150% and 200%.
200%-L (6.6992 μ g/mL)：Homopiperazine stock solution C；150%-L (5.0244 μ g/mL)：Precision pipettes
In 0.75mL homopiperazine stock solution C to 2mL sample introduction bottles, 0.25mL5% dilution in acetonitrile is added, shakes up；100%-L (3.3496 μ
g/mL)：Precision pipettes in 0.5mL homopiperazine stock solution C to 2mL sample introduction bottles, and 0.5mL5% dilution in acetonitrile is added, shakes up；
80%-L (2.6797 μ g/mL)：Precision pipettes in 0.4mL homopiperazine stock solution C to 2mL sample introduction bottles, and 0.6mL5% second is added
Nitrile dilutes, and shakes up；60%-L (2.0098 μ g/mL)：Precision pipettes in 0.3mL homopiperazine stock solution C to 2mL sample introduction bottles, adds
Enter 0.7mL5% dilution in acetonitrile, shakes up；40%-L (1.3398 μ g/mL)：Precision pipette 0.2mL homopiperazines stock solution C to 2mL into
In sample bottle, 0.8mL5% dilution in acetonitrile is added, shakes up；20%-L (0.6699 μ g/mL)：Precision pipettes the storage of 0.1mL homopiperazines
In standby liquid C to 2mL sample introduction bottles, 0.9mL5% dilution in acetonitrile is added, shakes up；LOQ-L(0.3350μg/mL)：Precision pipettes
In 0.05mL homopiperazine stock solution C to 2mL sample introduction bottles, 5% dilution in acetonitrile of 0.95mL is added, shakes up.
By embodiment 1 provide assay method, successively sample introduction measure, using peak area as ordinate, reference substance solution concentration
Standard curve is drawn for abscissa (μ g/mL), the result is shown in table 2, the homopiperazine standard curve of drafting is as shown in Figure 2.
2 homopiperazine standard curve of table
Embodiment 3
The sample-adding recovery test for the assay method that embodiment 1 provides
Method by being loaded recycling analyzes the accuracy of the assay method of the offer of embodiment 1, hydrochloric acid method is taken to relax
Ground that 15mg, it is accurately weighed, it is placed in 10mL volumetric flasks, parallel 11 parts, takes wherein 2 parts, the homopiperazine content in determination sample；
Wherein 3 parts are taken, adds 0.1mL homopiperazine stock solution B respectively, adds 5% acetonitrile constant volume and mixing, it is molten as 50% recovery of standard addition
Liquid；Wherein 3 parts are taken, adds 0.2mL homopiperazine stock solution B respectively, adds 5% acetonitrile constant volume and mixing, as 100% recovery of standard addition
Solution；Wherein 3 parts are taken, adds 0.3mL homopiperazine stock solution B respectively, adds 5% acetonitrile constant volume and mixing, as 150% mark-on reclaims
Rate solution is measured by the UPLC-MS methods of embodiment 1, the results are shown in Table 3, the results show that the homopiperazine rate of recovery is 93~119%, 9
The rate of recovery RSD of needle is 9%, shows that the assay method that embodiment 1 provides has good accuracy.
3 homopiperazine rate of recovery result of table
Embodiment 4
The precision test for the assay method that embodiment 1 provides
By the method for 100% sample-adding recycling, the precision of the assay method of the offer of embodiment 1 is analyzed, salt is taken
Sour Fasudil 15mg, it is accurately weighed, parallel 8 parts, wherein 2 parts are taken, the homopiperazine content in determination sample；Wherein 6 parts are taken, point
Not plus 0.2mL homopiperazine stock solution B, add 5% acetonitrile constant volume and mixing, as 100% recovery of standard addition solution, by embodiment 1
UPLC-MS methods measure, the results are shown in Table 4, the results show that the homopiperazine rate of recovery be 112~122%, 6 needle rate of recovery RSD be
4%, show that the assay method that embodiment 1 provides has good repeatability.
The repeated result of table 4
Embodiment 5
The specificity experiment for the assay method that embodiment 1 provides
Take 5% acetonitrile as blank solvent, reference substance solution and each 5 μ L of test solution in embodiment 1 are injected separately into
UPLC-MS is measured by the UPLC-MS methods of the present embodiment 1, is recorded chromatogram, as a result see Fig. 3,1 blank solvent of figure label,
Label 2 be embodiment 1 in reference substance solution, label 3 be embodiment 1 in test solution, the results showed that, blank solvent and
Test solution is noiseless to the measurement of homopiperazine.
, embodiment 6
The stability test for the assay method that embodiment 1 provides
Reference substance solution in Example 1, is placed at room temperature, stability of solution is investigated, by the UPLC- of embodiment 1
MS methods, sample introduction, records the peak area of homopiperazine respectively, and note calculates reference substance solution peak area RSD, the results are shown in Table 5, the results showed that 8h
Interior, the peak area RSD of reference substance solution is 2%, illustrates that the assay method that embodiment 1 provides is with good stability.
5 reference substance solution stability result of table
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although with reference to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution recorded in example is modified or equivalent replacement of some of the technical features.All essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (2)
1. a kind of method measuring homopiperazine content in Fasudic hydrochloride, which is characterized in that include the following steps：
S1, homopiperazine reference substance is taken, using 5% acetonitrile solution as solvent, prepares homopiperazine reference substance solution, hydrochloric acid method is taken to relax ground
You prepare test solution using 5% acetonitrile solution as solvent；
Two parts of S2, parallel preparation homopiperazine reference substance solutions are detected through UPLC-MS methods, obtain high piperazine in reference substance solution respectively
The peak area of piperazine calculates the ratio of the concentration of peak area and reference substance solution, obtains the response factor of homopiperazine；
S3, it takes test solution to be detected through UPLC-MS methods, obtains the peak area of test solution, calculated for examination with response factor
The content of homopiperazine in product solution.
2. a kind of method measuring homopiperazine content in Fasudic hydrochloride according to claim 1, which is characterized in that institute
The chromatographic condition for stating UPLC-MS methods in S2 steps and the S3 steps is：Using CSH C18 chromatographic columns (2.1 × 100mm, 1.7 μ
M), column temperature is 35 DEG C；5 μ L of sample size；Detector is mass detector, ion source ESI, positive ion mode, ion 101；
Using 0.1% formic acid as mobile phase A, acetonitrile is Mobile phase B, flow velocity 0.2mL/min；Gradient elution program is：0~1min, stream
The percentage by volume of dynamic phase B is 5%；1~5min, the percentage by volume of Mobile phase B is by 5% to 90%；5~5.1min, flowing
The percentage by volume of phase B is by 90% to 5%；The percentage by volume of 5.1~7min, Mobile phase B are 5%.
Gradient elution program
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Cited By (5)
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| CN110596293A (en) * | 2019-10-18 | 2019-12-20 | 山东威高药业股份有限公司 | High performance liquid detection method for homopiperazine |
| CN112748197A (en) * | 2020-12-23 | 2021-05-04 | 上海微谱化工技术服务有限公司 | Accurate quantitative determination method for impurity homopiperazine in medicine |
| CN113447584A (en) * | 2021-06-28 | 2021-09-28 | 山西省检验检测中心(山西省标准计量技术研究院) | Detection and analysis method for high piperazine in fasudil hydrochloride injection |
| CN115112800A (en) * | 2022-07-01 | 2022-09-27 | 河南润弘制药股份有限公司 | Improved detection method for high piperazine in fasudil hydrochloride injection |
| CN115267004A (en) * | 2022-08-09 | 2022-11-01 | 宣城菁科生物科技有限公司 | Method for detecting content of related substances in fusidic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110596293A (en) * | 2019-10-18 | 2019-12-20 | 山东威高药业股份有限公司 | High performance liquid detection method for homopiperazine |
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| CN115112800A (en) * | 2022-07-01 | 2022-09-27 | 河南润弘制药股份有限公司 | Improved detection method for high piperazine in fasudil hydrochloride injection |
| CN115112800B (en) * | 2022-07-01 | 2023-07-07 | 河南润弘制药股份有限公司 | Improved detection method for homopiperazine in fasudil hydrochloride injection |
| CN115267004A (en) * | 2022-08-09 | 2022-11-01 | 宣城菁科生物科技有限公司 | Method for detecting content of related substances in fusidic acid |
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