Development of a stability-indicating capillary electrophoresis method for norfloxacin and its inactive decarboxylated degradant |
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Authors: | Ahmed Alnajjar Abubakr M. Idris Hamed H. AbuSeada |
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Affiliation: | Department of Chemistry, College of Science, King Faisal University, Hofuf, Saudi Arabia |
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Abstract: | A simple, accurate, precise, rapid and sensitive stability-indicating capillary electrophoresis (CE) method was optimized and validated for the simultaneous determination of norfloxacin and its inactive decarboxylated degradant in pharmaceuticals. The univariant method was used to optimize electrophoretic factors including injection time, separation voltage and column temperature. Electrolyte concentration and pH were optimized using the factorial design and response surface methods. The optimum conditions obtained were: 10 mmol l− 1 phosphate at pH 2.5, hydrodynamic injection time of 8 s at pressure 0.5 p.s.i., separation voltage 25 kV and column temperature 25 °C. The separation was carried out into a fused-silica capillary column (31.2 cm length × 50 μm i.d.) with detection at 301 and 285 nm for the intact drug and the degradant, respectively using a diode array detector. For both analytes, the method enjoys wide dynamic range (1-50 μg ml− 1) with good detectability (limits of detection 0.11 μg ml− 1). In addition, acceptable accuracy (recovery > 95%); and good repeatability and intermediate precision (RSD < 3.5%) were obtained. |
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Keywords: | Capillary electrophoresis Pharmaceutical analysis Stability-indicating method Norfloxacin Experimental design methods |
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