Development and Validation of Chromatographic and Spectrophotometric Methods for the Quantitation of Rufinamide in Pharmaceutical Preparations

Abstract

Objectives: Two optimized and validated high performance liquid chromatography (HPLC) and spectrophotometric methods are proposed. The developed methods were quantified with high sensitivity, accuracy, and precision at low concentrations to determine rufinamide (RUF) in active pharmaceutical ingredients (API) and pharmaceutical preparations.

Materials and methods: HPLC method was developed using a base deactivated silica Hypersil C₁₈ column and a combination of methanol: acetonitrile: water (15: 10: 75, v/v/v) as the mobile phase and detected at 210 nm. A reaction of RUF with sodium nitrite and hydrochloric acid occurred, absorbed maximally at 385 nm was extended to develop a ultraviolet (UV)-visible spectrophotometric method to determine RUF in API and pharmaceutical preparations.

Results: Different analytical validation parameters, including specificity, linearity, accuracy, precision, the limit of detection, quantification, ruggedness, and robustness, were determined as per International Conference on Harmonization guidelines. The linearity range of RUF was 0.15-3.5 and 10-100 μg/mL for HPLC and spectrophotometric methods, respectively.

Conclusion: The proposed investigations were valuable for drug monitoring and regular analysis of RUF in quality control and research laboratories. Moreover, the accuracy and precision obtained with the UV-visible spectrophotometer implied that it could be a cheap, easy, and alternative method, while HPLC could be sensitive to determine RUF at low concentration levels.

Keywords: HPLC; Rufinamide; UV-visible spectrophotometry; quality control laboratories; validation.

Figure 1

Effect of concentration and error bars with standard deviations of HCl/ NaNO₂

Figure 2

Proposed reaction scheme

Figure 3

RUF chromatogram with a retention time of 4.65 min