title: Validated stability indicating LC method for carprofen: characterization of degradation products by MS.
abstract: A simple, sensitive, and selective stability indicating high performance liquid chromatographic method has been developed and validated for quantitative analysis of carprofen (CPF) in presence of its degradation products. All degradation products in acid hydrolysis and photolysis were separated, identified by mass spectroscopic method and probable structures were elucidated. The forced degradation studies were performed on a bulk sample of CPF by using various methods like 0.1 M hydrochloric acid, 0.1 M sodium hydroxide, 0.33% hydrogen peroxide (H(2)O), heating at 60°C and exposure to UV light at 254 nm. A 5 μm particle octa desyl silane (ODS) column (150 mm × 4.6 mm) was used with acetonitrile-ammonium acetate (100 mM, pH-6.7) 40:60 (v/v) as a mobile phase at flow rate of 1.2 mL/min. Column oven temperature was maintained at 30°C and quantitation was achieved at 239 nm on the basis of peak area. The linear range and correlation coefficient (r(2)) was found 0.5-60 μg/mL and 0.9999 respectively. The limit of detection (LOD) and limit of quantitation (LOQ) were obtained 0.066 μg/mL and 0.20 μg/mL respectively . The proposed method was found to be suitable and accurate for quantitative analysis, stability study and characterisation of degradation product of CPF.
authors.affiliation: Department of Chemistry, Shivaji University, Kolhapur, 416004, (MS), India.
authors.forename: Shahaji S
authors.initials: SS
authors.lastname: Tele
authors.forename: Tushar V
authors.initials: TV
authors.lastname: Gadkari
authors.forename: Shivajirao R
authors.initials: SR
authors.lastname: Patil
authors.forename: Govind B
authors.initials: GB
authors.lastname: Kolekar
mesh_terms: D002227:Carbazoles / Q000032:analysis* / Q000737:chemistry; D002853:Chromatography, Liquid / Q000379:methods*; D004355:Drug Stability; D016018:Least-Squares Analysis; D013058:Mass Spectrometry / Q000379:methods*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013696:Temperature
chemical_list: D002227:Carbazoles; C007005:carprofen