The goal of this project was to isolate and identify individual components from aircraft de‐icing/anti‐icing fluids (ADAs) through a toxicity‐based bioassay analysis. A Microtox® bioassay fractionation scheme was used to isolate a number of active fractions from ADAFs. Active fractions were identified using multiple spectral techniques, including nuclear magnetic resonance, gas chromatography–mass spectrometry, liquid chromatography–mass spectrometry, and ultraviolet characterization. The primary Microtox‐active fraction was shown to be a mixture of benzotriazole and tolyltriazoles, which are used as corrosion inhibitors in ADAF formulations. The identity of the compounds was confirmed through spectral and Microtox‐toxicity analysis and comparison of commercially available standards.

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Abstract-The goal of this project was to isolate and identify individual components from aircraft de-icing/anti-icing fluids (ADAFs) through a toxicity-based bioassay analysis. A Microtox bioassay fractionation scheme was used to isolate a number of active fractions from ADAFs. Active fractions were identified using multiple spectral techniques, including nuclear magnetic resonance, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, and ultraviolet characterization. The primary Microtox-active fraction was shown to be a mixture of benzotriazole and tolyltriazoles, which are used as corrosion inhibitors in ADAF formulations. The identity of the compounds was confirmed through spectral and Microtox-toxicity analysis and comparison of commercially available standards.

A strategy for expanding the linear working range in bioanalysis using quantitative high performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) is presented. The strategy involves monitoring multiple product ions. Herein we demonstrate the strategy on a rat plasma assay for a proprietary experimental drug where the linear range is expanded from 2 to 4 orders of magnitude. A primary sensitive ion was monitored to obtain a high sensitivity range calibration curve (0.400 to 100 ng/mL) while a less sensitive secondary ion was monitored to obtain a low sensitivity range calibration curve (90.0 to 4000 ng/mL). Each calibration curve gave acceptable linearity (r >0.990). Quality control samples at low, mid and high levels within each calibration curve demonstrated acceptable precision and accuracy (within 20% for all levels). The technique was successfully applied to rat pre-clinical sample analysis.