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

• UHPLC–DAD–HRESIMS method for detection of dehalogenation impurities in pharmaceuticals.
• Resolution and MS compatible detection with a perflurophenyl column and ACN/NH4HCO2 (pH 3.5) eluent.
• Lower resolution single quadrupole MS detector correctly identified potential dehalogenation impurities.
• Unambiguous identification of dehalogenation impurities or associated isomers by HRESI(+) detection.

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).

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