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Detection and Occurrence of Acrylamide in U.S. Foods. Steven M. Musser, Ph.D. Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration College Park, Maryland. Topics.
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Detection and Occurrence of Acrylamide in U.S. Foods Steven M. Musser, Ph.D. Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration College Park, Maryland
Topics • Development and performance of an LC/MS/MS method for the quantitation of acrylamide in a wide variety of foods • Results of exploratory survey data from U.S. foods
Method Highlights • Sample preparation • Sample size • Stable isotope labeled internal standard • Extraction with water • Two step solid phase extraction • Chromatography • Temperature controlled • Many columns tested, 3 found acceptable • Detection • Electrospray • Liquid Chromatography/Mass Spectrometry/Mass Spectrometry (LC/MS/MS)
Sample Preparation • Sample size used for extraction • 1 gram sub-sample Bread Crumbs (4) 63 ppb 1.5% RSD Cereal (4) 217 ppb 1.2% RSD Coffee (4) 127 ppb 3.9% RSD Potato Chips (4) 613 ppb 2.7% RSD • 4 gram sub-sample Bread Crumbs (3) 65 ppb 2.6% RSD Cereal (3) 214 ppb 5.2% RSD Coffee (3) 115 ppb 0.9% RSD Potato Chips (3) 597 ppb 4.8% RSD
OASIS SPE only With 2nd SPE step Sample Preparation
Phenomenex Hydro-RP YMC ODS H-80 Phenomenex Aqua C18 Chromatography
Quality Control • Recovery of internal standard • Duplicate analyses of samples • Reanalysis of randomly selected samples • Performance of standards • Signal/noise and ion abundance ratios
Method Performance • Linearity • 8 ppb to 3200 ppb • Response factor 0.98, s.d. 0.05% and RSD 4.6% • Recovery • 94.8% ± 5.6% • Precision Bread Crumbs (4) 63 ppb 0.9 1.5% RSD Cereal (4) 217 ppb 2.6 1.2% RSD Coffee (4) 127 ppb 4.9 3.9% RSD Potato Chips (4) 613 ppb 16.7 2.7% RSD
Proficiency Testing • National Food Processors Association • 5 Labs with LC/MS/MS • Crackers - 137 ppb mean =148 ppb, s.d.= 8.4 • Chips - 224 ppb mean = 225 ppb, s.d. = 13.4 • Food Analysis Performance Assessment Scheme (FAPAS) • Crispbread • 37 participants, 32 satisfactory scores • 22 (8) labs used LC/MS methods, 19 labs used GC/MS methods • Assigned value 1213 µg/kg • CFSAN reported value 1264 ug/kg
Additional Method Research Needs • Preparation of final report for single lab method validation • Preparation of proficiency test materials • Three lab peer verification of the method • Full multi-lab study • Inexpensive, accurate screening method • Survey foods in U.S.
Exploratory Survey of Acrylamide Levels in U.S. Foods • How foods were chosen • Previously reported • Recent unpublished findings • Consumption by group or total • Sampling is not representative • Many foods have one sample
Food Survey Progress • About 300 different food samples analyzed • Nearly 700 analyses • More than 35 different food types • Baby foods Nuts • Breads Seasonings • Coffee Vegetables • Meats
Baby food (fruit, cereal) Caramel Chicken (raw, cooked) Creamers, nondairy Fish (raw, cooked) Gelatin Gravy Infant Formula Marshmallows\ Milk (condensed) Potatoes (uncooked) Soy Sauce Frozen vegetables Vegetable protein Foods with Little or No Acrylamide (LOQ 10 ppb)
Consumer Preferences: Baked French Fries This is one example of the effect of personal preference. We should note for clarification that the levels of acrylamide shown here are on the low end of our observed range for frozen fries baked according to instructions (119 -1325 ppb, 12 products).
( 0 ppb) (11 ppb) (1326 ppb) (4885 ppb) Consumer Food Preparation
Concluding Remarks • The analytical method is reliable, and results are directly comparable to data from many other laboratories • There is considerable variability in acrylamide levels both in commercially produced and consumer produced foods • A number of factors contribute to the variability and small sample numbers could be misleading • The amount of variability observed in certain food types suggests it may be possible to reduce acrylamide levels