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J Pharm Biomed Anal. 2014 Jun;94:111-7. doi: 10.1016/j.jpba.2014.01.034. Epub 2014 Jan 31.

Water determination in active pharmaceutical ingredients using ionic liquid headspace gas chromatography and two different detection protocols.

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  • 1Department of Chemistry and Biochemistry, University of Texas at Arlington, TX, USA.
  • 2Department of Chemistry and Biochemistry, University of Texas at Arlington, TX, USA. Electronic address:


A rapid, accurate, precise and versatile analytical method was developed for the detection and quantification of water in solid active pharmaceutical ingredients (APIs). The headspace gas chromatography (HSGC) method utilized an ionic liquid (IL) based open tubular capillary GC column to increase sensitivity and ruggedness of this method. ILs are also utilized as the headspace solvent because of their low vapor pressure, unique physiochemical properties and high thermal stability. This method is not affected by side reactions and solubility problems which are common with Karl Fischer Titration (KFT) methods. Nor is it as limited as weight loss on drying approaches. The ability to use either/both modern thermal conductivity or barrier ion discharge GC detection provides flexibility, different dynamic ranges and sensitivity. The developed method also was shown to be broadly applicable.

Copyright © 2014 Elsevier B.V. All rights reserved.


Ionic liquid; Karl Fischer; Pharmaceuticals

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