Comparison of headspace-SPME-GC–MS and LC–MS for.pdf

Available online at Food Chemistry Food Chemistry 107 (2008) 1701–1709 /locate/foodchem Analytical Methods Comparison of headspace-SPME-GC–MS and LC–MS for the detection and quantification of coumarin, vanillin, and ethyl vanillin in vanilla extract products Lowri S. De Jager *, Gracia A. Perfetti, Gregory W. Diachenko Center for Food Safety and Applied Nutrition, US Food and Drug Administration, 5100 Paint Branch Parkway, College Park, MD 20785, United States Received 14 August 2007; received in revised form 25 September 2007; accepted 26 September 2007 Abstract A headspace-solid phase micro-extraction (HS-SPME) GC–MS method has been developed for the determination of coumarin, van- illin and ethyl vanillin in vanilla products. Limits of detection ranged from 1.33 to 13.2 ng mL1. Accuracy and precision data for the method were measured and compared to those obtained using LC-ESI-MS. A survey of 24 commercially available vanilla products was completed using both techniques. No coumarin was detected in any of the samples. Examination of the GC–MS chromatograms revealed the presence of 18 other flavor related compounds in the samples. The method validation and sample analysis data using HS-SPME-GC– MS were comparable to those obtained using the LC–MS method. Because the two methods are conceptually different from one another, both methods would not be su