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HomeSmall Molecules Analysis & QCSafinamide Impurity Profiling by HPLC Assay Methods

Safinamide Impurity Profiling by HPLC Assay Methods

Neil J. Williams1, Jenna Milliken1

MilliporeSigma

INTRODUCTION

A simple and accurate method was developed for purity analysis of safinamide using high-performance liquid chromatography with a diode array detector (HPLC-DAD). The method was developed for a family of safinamide compounds consisting of the active pharmaceutical ingredient safinamide and multiple corresponding impurities. This is to our knowledge the first reported method for safinamide and related impurities. Safinamide free acid, safinamide mesylate, safinamide defluor-derivative, and safinamide imidazolidinone can be resolved in a 20-minute method using an Ascentis® Express C8 column (150 x 4.6 mm, 5 μm). A gradient that utilized 0.1% trifluoroacetic acid in water and acetonitrile was employed. Under the applied conditions the system suitability criteria are met. The method demonstrates good resolution and selectivity, reproducibility, and sensitivity.

Chemical structures for Safinamide Free Acid, Safinamide Mesylate, Safinamide Deflour-Derivative, and Safinamide Imidazolidinone

Safinamide Free Acid
PHR2380

Safinamide Mesylate
PHR2379

Safinamide Deflour-Derivative
PHR2381

Safinamide Imidazolidinone
PHR2382

EXPERIMENTAL CONDITIONS

Results

Blank chromatogram

Figure 1.Blank chromatogram.

Chromatogram for Safinamide Mesylate System Suitability Solution

Figure 2.Chromatogram for safinamide mesylate system suitability solution.

Chromatogram for Resolution Solution of safinamide and its 3 related impurities

Figure 3.Chromatogram for resolution solution.

Chromatographic Data - Specificity (Resolution Solution)

Linearity - Calibration

Calibration curve of Safinamide Mesylate

Figure 4.Calibration curve of safinamide mesylate.

Calibration curve of Safinamide Free Acid

Figure 5.Calibration curve of safinamide free acid.

Calibration curve of Safinamide Defluro-Derivative

Figure 6.Calibration curve of safinamide defluro-derivative.

Calibration curve of Safinamide Imidazolidinone

Figure 7.Calibration curve of safinamide imidazolidinone.

CONCLUSION

A new method was developed for analyzing the purity of safinamide and its related compounds using high-performance liquid chromatography with a diode array detector. The method uses an Ascentis® Express C8 HPLC column and a gradient of 0.1% trifluoroacetic acid in water and acetonitrile and takes 20 minutes to resolve the compounds. The method is reproducible and sensitive and shows good resolution and selectivity.

See also Small Molecules Analysis & Quality Control (QC) for more information on other applications or use our chromatogram search.

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