Method for simultaneous detection of genotoxic impurities methyl 5-isoquinolinesulfonate and ethyl 5-isoquinolinesulfonate in fasudil hydrochloride
The technology of methyl isoquinoline sulfonate and ethyl isoquinoline sulfonate is applied in the field of detection of genotoxic impurities in fasudil hydrochloride, and achieves the effects of low detection cost, high sensitivity and improved sensitivity
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0047]Example 1, the determination of the HPLC detection method of the present invention
[0048]UV spectrum scanning of 5-isoquinolysulfonate and 5-isoquinolysulfonate: Precision 5-isoquinolysulfonate and 5-isoquinolysulfonate control The acetonitrile is dissolved and diluted to prepare a solution containing 5- isoquinolysulfonate and 5- μg / ml of ethyl ester. Each solution was taken in the range of 400 nm to 200 nm, and the results are shown in Table 1.
[0049]Table 1 5- Maximum absorption wavelength of methyl isoquinolysulfonate and 5-isoquinolysulfonate
[0050] name Maximum absorption wavelength 5- isoquinolysulfonate A238.00NM 5- isoquinolysulfonate A238.00NM Blank solvent /
[0051]It can be seen that the 5-isoquinoline sulfonate and 5-isoquinolin sulfonate have a large absorption at the vicinity of 238 nm, indicating 5-isoquinoline sulfonate and 5-isoquinoline. Ethyl sulfonate can be selected from the UV detector, and 238 nm can be selected as the detection wavelength.
[0052]The ...
Embodiment 2
[0072]Example 2, Separation and Determination of Michloric Toxic Impact of Hydrochloric Acid in Test
[0073]1, formulation of related solutions
[0074](1) 5-isoquinoline sulfonate reservoir: Take 5-isoquinoline sulfonate, surely, precisely weighted, dissolved with methanol and quantitatively dilute each 1 μg of solution, as 5 - Isoquinolysulfonate reservoir.
[0075](2) 5-isoquinolysulfonate inlate: 5-isoquinolysulfonate aliquots, precision weighing, dissolved with methanol and quantitatively dilute to prepare 1 μg of solution containing 1 μg, as 5 - Isoquinolysulfonate inlate.
[0076](3) Systematic Solution: Take the hydrochloric acid method (Source: China Food Pharmaceutical Authority Research Institute Bottom: 100614-201603) About 50mg, precision weighing, set 10mL volumetric flask, add diluent to the amount of dissolution 5-isoquinoline sulfonate and 5-isoquinolin sulfonate storage fluid 0.8 ml, diluted with a diluent, and shake well as a systematic solution.
Embodiment 3
[0093]Example 3, linear relationship test
[0094]Take 5-isoquinoline sulfonate and 5-isoquinoline sulfonate control material, and the plus-in-phase A dilution is diluted to prepare a solution of about 1 μg of each of the respective plactions, as a linear reserve; The amount of linear reservoir is applied, and the plus-in phase A is diluted to form a solution, 0.04 μg / ml, 0.08 μg / ml, 0.12 μg / mL, 0.16 μg / ml, concentration solution, as each concentration linear solution.
[0095]A 20 μl injection liquid chromatography is obtained by precision, respectively, and the chromatogram is recorded. The peak area (a) of concentration C (μg / ml) is shown in Table 5 and Table 6.
[0096]Table 5- Linear results of methyl isoquinolysulfonate
[0097]
[0098]Table 6 5- Isoquinolin sulfonate linear results
[0099]
[0100]It can be seen from Table 5, and 5-isoquinolin sulfonate is in the concentration range of 0.01374 μg / mL to 0.16584 μg / ml, linear relationship, linear equation is: y = 157.3308X-0.3437, R...
PUM
| Property | Measurement | Unit |
|---|---|---|
| wavelength | aaaaa | aaaaa |
| concentration | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More