Method for separating and determining two genotoxic impurities in topiromilast
A method of determination and genotoxicity technology, applied in the field of analysis and detection, can solve the problems of no impurity detection literature reports, etc., and achieve the effect of ensuring safety
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Embodiment 1
[0043] (1) Solution preparation: 1% phosphoric acid-acetonitrile (90:10) as the diluent; take an appropriate amount of topirast, accurately weighed, put it in a volumetric flask, add diluent to dissolve and dilute to make The solution of piridast 1mg is used as the test solution; each appropriate amount of TP02-IMP-A and TP-IMP-A reference substance is taken respectively, accurately weighed, placed in a volumetric flask, dissolved with a diluent and made into each ml A solution containing 10 ng of both TP02-IMP-A and TP-IMP-A was used as a reference solution.
[0044] (2) Precisely measure 50 μl each of the test solution and the reference solution, inject them into the high-performance liquid chromatograph respectively, and record the chromatogram. The conditions of the high-performance liquid chromatograph are:
[0045] Chromatographic column: Octadecylsilane bonded silica gel as filler, 250*4.6mm, 5μm;
[0046] Column temperature: 30°C;
[0047] Detection wavelength: 220nm...
Embodiment 2
[0052] Example 2 System suitability test for detecting two genotoxic impurities in topirast
[0053] Take an appropriate amount of topiralast, TP02-IMP-A and TP-IMP-A reference substances respectively, place them in a volumetric flask, dissolve them with a diluent and make each ml containing 1mg of topiralast, containing TP02-IMP- A and TP-IMP-A are both 10ng solutions, as a system suitability solution. Precisely measure 50 μl, inject it into the liquid chromatograph, and record the chromatogram, such as figure 1 shown. The peaks of TP02-IMP-A, TP-IMP-A and topiralast elute sequentially, and the resolution between adjacent chromatographic peaks is not less than 1.5. The test results are as follows:
[0054] .
[0055] Using the above method, the two genotoxic impurities TP02-IMP-A and TP-IMP-A in topirax and topiralast can be detected, and the peak separation of these three are all>1.5, also That is to say, the method can well separate TP02-IMP-A, TP-IMP-A and topiramat...
Embodiment 3
[0056] Example 3: Limit of Quantitation Test for Two Genotoxic Impurities in Topirast
[0057] Take an appropriate amount of TP02-IMP-A and TP-IMP-A reference substances respectively, place them in a volumetric flask, dissolve them with a diluent and make a solution containing 10 ng of TP02-IMP-A and TP-IMP-A per ml , gradually diluted with a diluent until the S / N is no less than 10.0, and the solution with this concentration was used as the limit of quantitation solution, and six parallel preparations were made. Precisely measure 50 μl of each solution, inject them into the liquid chromatograph respectively, and record the chromatograms. The test results are as follows:
[0058] .
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