title: Characterization of the Oxidative Degradation Product of Darunavir by LC-MS/MS.
abstract: A rapid, selective, and reliable LC-MS(n) method has been developed and validated for the isolation and structural characterization of the degradation product of darunavir (DRV). DRV, an HIV-1 protease inhibitor, was subjected to intrinsic oxidative stress conditions using 30% hydrogen peroxide and the degradation profile was studied. The oxidative degradation of DRV resulted in one degradation product. The unknown degradation product was separated on a Hibar Purospher C18 (250 mm × 4.6 mm; 5 µm) column by using 0.01 M ammonium formate (pH 3.0) and acetonitrile as mobile phase in the ratio of 50:50, v/v. The eluents were monitored at 263 nm using a UV detector. The isolated degradation product was characterized by UPLC-Q-TOF and its fragmentation pathway was proposed. The proposed structure of the degradation product was confirmed by HRMS analysis. The developed stability-indicating LC method was validated with respect to accuracy, precision, specificity/selectivity, and linearity. No prior reports were found in the literature about the oxidative degradation behavior of DRV.
authors.affiliation: Department of Pharmaceutical Analysis, JSS College of Pharmacy, [A Constituent College of JSS University, Mysore], Udhagamandalam, Tamilnadu-643001, India.
authors.forename: Karthik
authors.initials: K
authors.lastname: Yamjala
authors.affiliation: Department of Pharmaceutical Analysis, JSS College of Pharmacy, [A Constituent College of JSS University, Mysore], Udhagamandalam, Tamilnadu-643001, India.
authors.forename: Jeevitha
authors.initials: J
authors.lastname: Atukuri
authors.affiliation: Department of Pharmaceutical Analysis, JSS College of Pharmacy, [A Constituent College of JSS University, Mysore], Udhagamandalam, Tamilnadu-643001, India.
authors.forename: Krishnaveni
authors.initials: K
authors.lastname: Nagappan
authors.affiliation: Department of Pharmaceutical Analysis, JSS College of Pharmacy, [A Constituent College of JSS University, Mysore], Udhagamandalam, Tamilnadu-643001, India.
authors.forename: Nivedeetha
authors.initials: N
authors.lastname: Halekote Shivaraju
authors.affiliation: Department of Pharmaceutical Analysis, JSS College of Pharmacy, [A Constituent College of JSS University, Mysore], Udhagamandalam, Tamilnadu-643001, India.
authors.forename: Meyyanathan
authors.initials: M
authors.lastname: Subramania Nainar
keywords: Characterization; Darunavir; Oxidative degradation; Validation
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