Abstract:

A highly sensitive method for the determination of genotoxic impurity 2-aminopyridine in Piroxicam employing hyphenated techniques have been presented. 2-aminopyridine was determined by LC-MS/MS method in selected ion monitoring mode (SIM) using LiChrospher RP-18 (100×4.6mm) 5.0 µm column. Gradient technique was applied for the elution of analytes using acetonitrile (mobile phase A) and 0.01M ammonium acetate buffer (mobile phase B) in different ratios. The gradient program (T/%B) was set as 0/5,2.50/15, 5.00/30, 10.00/50, 15.00/95, 20.00/95. Developed method was validated as per International Conference on Harmonization guidelines. The LOD and LOQ values found for 2-aminopyridine were 5.25 ppm and 75 ppm. Method has accuracy within 97 -103.4% for the analyte. This method is a good quality control tool for quantitation of 2-aminopyridine impurity at very low levels in Piroxicam.

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