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HomeSmall Molecule HPLCFingolimod HPLC Assay and Impurity Profiling Methods Following United States Pharmacopeia Monograph Guidelines

Fingolimod HPLC Assay and Impurity Profiling Methods Following United States Pharmacopeia Monograph Guidelines Using a Purospher STAR C18 Column and UV Detection

Introduction

A rapid, accurate, and simple method was implemented for the total chromatographic purity analysis of Fingolimod Hydrochloride by High Performance Liquid Chromatography equipped with a Diode Array Detector. The experimental conditions follow guidelines, with minor allowed modifications, from the USP43-NF38 monograph methods for Fingolimod Hydrochloride Assay and Organic Impurities Profiling. Fingolimod hexyl homolog, Fingolimod heptyl homolog, Fingolimod Hydrochloride, Fingolimod nonyl homolog, Fingolimod decyl homolog, 3-Phenethyl Fingolimod analog, and 2-Phenethyl Fingolimod analog can be resolved with baseline separation utilizing the USP‘s 33-minute gradient method and a Purospher STAR RP-18 HPLC column (150 x 3.0 mm, 3 μm). A 0.1% solution of Phosphoric acid in water and acetonitrile were employed as the mobile phases for the gradient elution. Under applied conditions, system suitability criteria are met, and the method demonstrates good resolution/selectivity, reproducibility, and sensitivity.

Chemical Structures

Fingolimod HCl

Figure 1.Fingolimod HCl

Fingolimod Hexyl Homolog

Figure 2.Fingolimod Hexyl Homolog

FingolimodHeptyl Homolog

Figure 3.FingolimodHeptyl Homolog

O-Acetyl Fingolimod

Figure 4.O-Acetyl Fingolimod

Fingolimod Nonyl Homolog

Figure 5.Fingolimod Nonyl Homolog

Fingolimod Decyl Homolog

Figure 6.Fingolimod Decyl Homolog

Fingolimod 3-Phenethyl Analog

Figure 7.Fingolimod 3-Phenethyl Analog

Fingolimod 2-Phenethyl Analog

Figure 8.Fingolimod 2-Phenethyl Analog

Experimental Conditions

Chromatographic Data (System Suitability Solution)

Specificity (System Suitability Solution)

Repeatability (System Suitability Solution)

Materials
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