Ruggedness testing of an HPLC method for the determination of ciprofloxacin

Abstract

The possibility of optimization of an HPLC method for the determinations of ciprofloxacin and ciprofloxacin impurity C was investigated according to the British Pharmacopoeia, using ruggedness testing. Four factors were selected to be tested in this ruggedness test (temperature of the column, volume of acetonitrile in the mobile phase, volume of the aqueous phase in the mobile phase and pH of the aqueous phase in the mobile phase). Seven responses were determined in each design experiment: retention times, peak heights, peak widths, number of theoretical plates, peak areas, peak areas RSD (%) and selectivity. A three-level design was used. The optimal conditions for the chromatographic procedure determined as the result of ruggedness testing were: pH of the aqueous phase in the mobile phase 3.0, column temperature 42 ºC and the acetonitrile to aqueous ratio in the mobile phase 14: 86 (v/v). The HPLC method using the optimal conditions was tested for selectivity linearity, precision, accuracy, limit of quantitation and limit of detection. The applicability of the suggested method was, as well, tested on the stability of ciprofloxacin in pharmaceutical preparations (tablets and infusion solution, products of Zdravlje-Pharmaco, Serbia) under stress stability data.

Keywords

• ciprofloxacin
• ciprofloxacin impurity c
• ruggedness test
• determination
• stability