Stability-Indicating Micellar LC Methods with Time-Programmed UV Detection for Determination of Three Oxicams in Pharmaceuticals with Direct Injection of Gel and Suppositories

Abstract

Two stability-indicating micellar liquid chromatographic methods were developed and validated for the determination of three oxicams, namely piroxicam (PX), tenoxicam (TX), and lornoxicam (LX), in presence of their degradation product and potential impurity (2-aminopyridine, AP). The analyses were achieved using C₈ column (150 mm × 4.6 mm i.d., 5 µm particle size). In Method I, a micellar mobile phase consisting of 0.15 M SDS, 10% n-propanol, 0.3% triethylamine, and 0.02 M orthophosphoric acid (pH 3.0) was used for simultaneous determination of PX, TX, and AP. In Method II, a mobile phase of the same composition but at pH 6.0 was used for separation of LX and AP. Time-programmed UV detection was applied to allow sensitive determination of the drugs and AP. Method I showed good linearity for PX, TX, and AP over the concentration ranges of 1.0–32.0, 1.0–20.0, and 0.5–10.0 µg/mL, respectively, while Method II was linear over the concentration ranges of 0.8–32.0 and 0.5–10.0 µg/mL for LX and AP, respectively. The developed methods were applied for quality control of the three drugs in pharmaceutical preparations including gel and suppositories with direct injection of samples. The proposed method agreed well with the concept of green chemistry.

Keywords:

• 2-aminopyridine
• formulations
• MLC
• oxicams
• stability-indicating

Notes

^a Each result is the average of three separate determinations.

^b n = 6.

^c n = 3.

^d Tabulated t and F values = 2.36 and 5.79, respectively.^{[ 46 ]}

^a Each result is the average of three separate determinations.

^a Calculations were done according to USP guidelines.^{[ 3 ]}

^a Each result is the average of three independent determinations.

^b n = 3.

^c Tabulated t and F values = 2.78 and 19.0, respectively.^{[ 46 ]}