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LC—MS/MS Studies for the Identification and Characterization of Degradation Products of Fenofibrate and Their Degradation Pathways

Mulgund S. V., Anbazhegan S., Gabhe S. Y.

Acta Chromatographica

2016

Vol. 28, no. 2

159--173

In the present study, the degradation behavior of Fenofibrate under different International Conference on Harmonization (ICH) suggested conditions was studied. Characterization of degradation products by liquid chromatography–tandem mass spectrometry (LC–MS/MS) studies in solution form was done, and the possible mechanism for the formation of degradants is discussed. Fenofibrate was subjected to different hydrolytic stress conditions and thermal stress condition (in solid form). Successful separation of drug from degradants was achieved on a C18 column using water–acetonitrile (25:75 v/v) as the mobile phase. Other high-performance liquid chromatography (HPLC) parameters were: flow rate, 1 mL min−1; detection wavelength, 286 nm; column temperature, 25 °C; and injection volume, 20 μL. The method was validated for linearity, precision, accuracy, robustness, and specificity and was stability-indicating one, based on the specificity studies. The drug degraded under acidic, basic, and oxidative hydrolytic stress while it was relatively stable towards neutral hydrolysis and thermal stress. The stressed samples were subjected to LC–MS/MS analysis. On the basis of spectral data, the structures of four degradation products and one interaction product were suggested. Degradation products were characterized to be isopropyl acetate, 2-[4-(4-chlorobenzoyl)phenoxy]-2-methyl propanoic acid, 4-hydroxy benzoic acid, and benzoic acid. The structure of one interaction product was proposed as methyl 2-[4-(4-chlorobenzoyl)phenoxy]-2-methylpropanoate.

Simultaneous HPTLC analysis of aspirin, atorvastatin calcium and clopidogrel bisulphate in the bulk drug and in capsules

Londhe S. V, Mulgund S. V, Deshmukh R. S, Jain K. S

Acta Chromatographica

2010

Vol. 22, no. 2

297--305

A simple, precise, and accurate HPTLC method has been established for simultaneous quantification of aspirin, atorvastatin calcium and clopidogrel bisulphate in the bulk drug and in a capsule dosage form. Chromatographic separation of the drugs was performed on aluminium foil plates precoated with silica gel 60 F 254 , with toluene-methanol-formic acid 6.5:3.5:0.1 ( v / v ) as mobile phase. Densitometric evaluation of the separated zones was performed at 254 nm. The three drugs were satisfactorily resolved with R F ± SD values 0.26 ± 0.01, 0.47 ± 0.01, and 0.78 ± 0.01 for aspirin, atorvastatin calcium, and clopidogrel bisulphate, respectively. The method was validated for linearity, specificity, accuracy, precision, and robustness, in accordance with ICH guidelines. Results from recovery studies indicated acceptable recovery of the drugs from the capsule dosage form. The intra-day and inter-day relative standard deviations were in the ranges 0.17–0.73% and 0.46–1.03% for aspirin, 0.36–0.87% and 0.44–0.62% for atorvastatin calcium, and 0.25–0.69% and 0.35–0.94% for clopidogrel bisulphate. The method proved to be a rapid and cost-effective quality-control tool for routine simultaneous analysis of aspirin, atorvastatin calcium, and clopidogrel bisulphate in the bulk drug and in a capsule formulation.