Determination of coumarin, vanillin, and ethyl vanillin in vanilla extract products: liquid chromatography mass spectrometry method development and validation studies

A LC–MS method was developed for the determination of coumarin, vanillin, and ethyl vanillin in vanilla products. Samples were analyzed using LC–electrospray ionization (ESI)–MS in the positive ionization mode. Limits of detection for the method ranged from 0.051 to 0.073 μg mL−1. Using the optimized method, 24 vanilla products were analyzed. All samples tested negative for coumarin. Concentrations ranged from 0.38 to 8.59 mg mL−1 ( x ¯ = 3.73 ) for vanillin and 0.33 to 2.27 mg mL−1 ( x ¯ = 1.03 ) for ethyl vanillin. The measured concentrations are compared to values calculated using UV monitoring and to results reported in a similar survey in 1988. Analytical results, method precision, and accuracy data are presented.