Challenging pharmaceutical analyses by gas chromatography with vacuum ultraviolet detection.

Vacuum ultraviolet (VUV) detector for gas chromatography (GC) provides qualitative spectral information from 125 nm to 240 nm. In this article, this information was applied to facilitate the development of a GC method for challenging pharmaceutical applications. Seven organic solvents were screened for trace level water content using VUV detection at 168 nm, and the results were used to identify n-hexane as a suitable diluent for 4-ethoxy-1,1,1-trifluoro-3-buten-2-one (ETFBO), a water reactive compound. Selective detection of compounds of interest was demonstrated by varying detection wavelengths. All compounds were detected at 145 nm except for one unknown impurity, which co-eluted with n-hexane solvent. This impurity was detected at 225 nm, where n-hexane has no absorbance. In addition, the VUV spectra were used to: 1) accurately track peaks during early method development; 2) detect co-eluting peaks; 3) match peak identity in a sample vs. a standard; and 4) assess peak purity. With the universal detectability, qualitative spectral information and ease of use, VUV will become a versatile tool for GC for both method development and routine analysis.