Detection of dehalogenation impurities in organohalogenated pharmaceuticals by UHPLC-DAD-HRESIMS

Erik L Regalado; Renee K Dermenjian; Leo A Joyce; Christopher J Welch

doi:10.1016/j.jpba.2013.12.043

Detection of dehalogenation impurities in organohalogenated pharmaceuticals by UHPLC-DAD-HRESIMS

J Pharm Biomed Anal. 2014 Apr:92:1-5. doi: 10.1016/j.jpba.2013.12.043. Epub 2014 Jan 7.

Authors

Erik L Regalado¹, Renee K Dermenjian², Leo A Joyce², Christopher J Welch³

Affiliations

¹ Merck Research Laboratories, Rahway, NJ 07065, USA. Electronic address: [email protected].
² Merck Research Laboratories, Rahway, NJ 07065, USA.
³ Merck Research Laboratories, Rahway, NJ 07065, USA. Electronic address: [email protected].

PMID: 24469094
DOI: 10.1016/j.jpba.2013.12.043

Abstract

The presence of dehalogenated impurities is often observed in halogen-containing pharmaceuticals, and can present a difficult analytical challenge, as the chromatographic behavior of the halogenated drug and the hydrogen-containing analog can be quite similar. In this study we describe the chromatographic separation and unambiguous identification of dehalogenation impurities or associated isomers in organohalogenated pharmaceuticals using UHPLC with a pentafluorophenyl column coupled with diode-array and high resolution electrospray ionization mass spectrometry detection (UHPLC-DAD-HRESIMS).

Keywords: Dehalogenation impurities; HRMS; Method development; Perfluorophenyl; UHPLC.

Publication types

Research Support, Non-U.S. Gov't

MeSH terms

Chromatography, High Pressure Liquid / methods*
Drug Contamination
Halogenation
Halogens / chemistry*
Pharmaceutical Preparations / chemistry*
Spectrometry, Mass, Electrospray Ionization / methods*

Substances

Halogens
Pharmaceutical Preparations