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There is a growing need to develop mass spectrometric methods for the characterization of oil sands naphthenic acids (structural formulae described by C_nH_2n+zO₂ where n is the number of carbon atoms and “z” is referred to as the “hydrogen deficiency” and is equal to zero, or is a negative, even integer) present in environmental samples. This interest stems from the need to better understand their contribution to the total acid number of oil sands acids; along with assessing their toxicity in aquatic environments. Negative‐ion electrospray ionization has emerged as the analytical technique of choice. For infusion samples, matrix effects are particularly evident for quantification in the presence of salts and co‐elutants. However, such effects can be minimized for methods that employ chromatographic separation prior to mass spectrometry (MS) detection. There have been several advances for accurate identification of …