Thermo Scientific Hypercarb Columns

F OOD S AFETYApplication NotesNominal Mean Conc. % Rel. Number of(ng/mL) (ng/mL) Error % CV Replicates0.250 0.253 1.1 12.1 50.500 0.485 -2.9 6.7 51.00 1.00(4) 0.4 4.6 55.00 4.86 -2.7 0.9 510.0 10.2 2.1 0.7 5100 101 0.7 0.5 5500 512 2.4 0.8 31000 1006 0.6 0.6 32500 2481 -0.8 0.6 3Table 1: Statistical data for the calibration curve of acrylamideTo monitor the consistency and reproducibility of thecolumn-switching LC-MS/MS method, a 1 ng/mL acrylamidestandard was analyzed immediately following eachfood sample. An example of this quality control standardanalyzed after the Potato Chip 2 sample is shown in Figure 5.Although the baseline for the m/z 72 → 55 SRM transitionis somewhat elevated near the retention time for acrylamide,the calculated concentration for this standard is 0.99 ng/mL,equating to a relative error of -1.0%.Table 2 reports the results for four different food samplesthat were assayed for acrylamide using the column-switchingLC method and MS/MS detection. The acrylamide concentrationsin each food sample were calculated by multiplyingthe measured solution concentration from duplicate injectionsby the extraction volume and dividing by the food samplemass that was extracted. The determined acrylamideconcentrations correlated well to those reported elsewherefor these classes of food. 1-5Potato PotatoCereal 1 Cereal 2 Chip 1 Chip 2Injection 1 17.17 ng/mL 55.93 ng/mL 57.11 ng/mL 29.18 ng/mLInjection 2 17.00 ng/mL 56.18 ng/mL 56.52 ng/mL 29.14 ng/mLMean 17.09 ng/mL 56.06 ng/mL 56.82 ng/mL 29.16 ng/mLExtraction Vol. 20.0 mL 20.0 mL 20.0 mL 20.0 mLMass Sample 2.003 g 2.007 g 2.021 1.995Acrylamide Conc. 171 ng/g 559 ng/g 562 ng/g 292 ng/gTable 2: Results of acrylamide assay from food samplesFigure 4: SRM chromatograms of the Potato Chip 2 sampleaqueous extractFigure 5: 1 ng/mL acrylamide standard analyzed directly after duplicateinjections of the aqueous extract of the Potato Chip 2 sampleConclusionsAn LC-MS/MS method has been developed for the measurementof acrylamide on the TSQ Quantum Discovery. UsingAPCI for the analysis of acrylamide from 100% water, anLOQ of 0.25 ng/mL acrylamide or 2.5 pg on column wasachieved. Incorpo ration of a column-switching LC methodprior to MS/MS detection of acrylamide eliminated the needto purify food sample extracts by SPE. The method wassuccessfully demonstrated for the analysis of four brands offood samples using TSQ Quantum Discovery in conjunctionwith a column-switching LC method.References1. Tareke, E.; Rydberg, P.; Karlsson, P.; Eriksson, S.; Tornqvist, M.J. Agric. Food Chem., 2002, 50, 4998-5006.2. Rosen, J.; Hellenas, K. Analyst, 2002, 127, 880-882.3. Musser, S. M. http://www.cfsan.fda.gov/~dms/acrylami.html4. Becalski, A.; Lau, B.P.; Lewis, D., Seaman, S.W. J. Agric. Food Chem.,2003, 51, 802-808.5. Brandl, F.; Demiani, S.; Ewender, J.; Franz, R.; Gmeiner, M.; Gruber, L.;Gruner, A.; Schlummer, M.; Smolic, S.; Stormer, A.; Wolz, G. Electron. J.Environ. Agric. Food Chem., 2002, 1(3), 1-8.6. Castle, L.; Campos, M.J.; Gilbert, J. J. Sci. Food Agric. 1993, 54,549-555.7. Ikonomou, M.G.; Blades, A.T.; Kebarle, P. J. Am. Soc. Mass Spectrom.,1991, 2, 497-505.8. McHale, K.J.; Winnik, W.; Paul, G. Proceedings of the 51st ASMSConference on Mass Spectrometry and Allied Topics, Montreal, 2003.22