Characterization of Oxidative Degradation Product of Darunavir by LC-MS/MS

YAMJALA, Karthik; ATUKURI, Jeevitha; NAGAPPAN, Krishnaveni; SHIVARAJU, Nivedeetha HALEKOTE; NAINAR, Meyyanathan SUBRAMANIA

doi:10.3797/scipharm.1505-10

Open AccessArticle

Characterization of Oxidative Degradation Product of Darunavir by LC-MS/MS

by

Karthik YAMJALA

,

Jeevitha ATUKURI

,

Krishnaveni NAGAPPAN

^*,

Nivedeetha HALEKOTE SHIVARAJU

and

Meyyanathan SUBRAMANIA NAINAR

Department of Pharmaceutical Analysis, JSS College of Pharmacy, [A Constituent College of JSS University, Mysore], Udhagamandalam, Tamilnadu-643001, India

^*

Author to whom correspondence should be addressed.

Sci. Pharm. 2015, 83(4), 623-633; https://doi.org/10.3797/scipharm.1505-10

Submission received: 15 May 2015 / Accepted: 30 June 2015 / Published: 30 June 2015

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Abstract

A rapid, selective, and reliable LC-MSⁿ 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.

Keywords: Characterization; Darunavir; Oxidative degradation; Validation

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MDPI and ACS Style

YAMJALA, K.; ATUKURI, J.; NAGAPPAN, K.; SHIVARAJU, N.H.; NAINAR, M.S. Characterization of Oxidative Degradation Product of Darunavir by LC-MS/MS. Sci. Pharm. 2015, 83, 623-633. https://doi.org/10.3797/scipharm.1505-10

AMA Style

YAMJALA K, ATUKURI J, NAGAPPAN K, SHIVARAJU NH, NAINAR MS. Characterization of Oxidative Degradation Product of Darunavir by LC-MS/MS. Scientia Pharmaceutica. 2015; 83(4):623-633. https://doi.org/10.3797/scipharm.1505-10

Chicago/Turabian Style

YAMJALA, Karthik, Jeevitha ATUKURI, Krishnaveni NAGAPPAN, Nivedeetha HALEKOTE SHIVARAJU, and Meyyanathan SUBRAMANIA NAINAR. 2015. "Characterization of Oxidative Degradation Product of Darunavir by LC-MS/MS" Scientia Pharmaceutica 83, no. 4: 623-633. https://doi.org/10.3797/scipharm.1505-10

APA Style

YAMJALA, K., ATUKURI, J., NAGAPPAN, K., SHIVARAJU, N. H., & NAINAR, M. S. (2015). Characterization of Oxidative Degradation Product of Darunavir by LC-MS/MS. Scientia Pharmaceutica, 83(4), 623-633. https://doi.org/10.3797/scipharm.1505-10

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Characterization of Oxidative Degradation Product of Darunavir by LC-MS/MS

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