S chneider & A ndersen : J ournal of AOAC I nternational V ol . 98, N o . 3, 2015  669

with responses above the 0.5 µg/kg calibrant for three or four residues. At the 0.90 µg/kg concentration, eight analytes (2%) generated peak areas below the response for the 0.5 extracted matrix calibrant. Based on the single point calibrant, these eight would yield residue concentrations in the range of 0.39 to 0.48 µg/kg. Some incurred samples were screened below the 0.5 µg/kg extracted matrix calibrant, but most of these had mean residue concentrations below 0.4 µg/kg, making it reasonable that these samples would be screened below the 0.5 µg/kg matrix calibration level. One MG in shrimp “incurred” sample yielded an estimated concentration of 0.44 µg/kg, yet the MG incurred shrimp mean concentration was 0.71 µg/kg.

Anna Hawkins, Shristi Prakash, and Michael Conway, OMIC USA Inc., Portland OR Jason Smith and Ross Potter, Canadian Food Inspection Agency, Dartmouth Laboratory, Dartmouth, Nova Scotia, Canada Robert Burger, U.S. Food and Drug Administration, Office of Regulatory Affairs, Denver Laboratory, Denver, CO Yanxuan Tina Cai, U.S. Food and Drug Administration, Office of Regulatory Affairs, Northeast Regional Laboratory, Jamaica, NY Andrew Fong, John Kibbey, and Chris Baker, U.S. Food and Drug Administration, Office of Regulatory Affairs, Arkansas Regional Laboratory, Jefferson, AR Andrew Harris and Linda Lissemore, University of Guelph, Laboratory Services, Chemistry Unit, Guelph, Ontario, Canada Sara Lupton, U.S. Department of Agriculture, Agricultural Research Service Biosciences Research Laboratory, Fargo, ND Haejung An, U.S. Food and Drug Administration, Office of Regulatory Affairs, Pacific Regional Laboratory Southwest, Irvine, CA  (1) Foster, F.J., &Woodbury, L. (1936) Progr. Fish Cult. 3 , 7–9.[7:TUOMGA]2. 0.CO;2  (2) Alderman, J. (1985 ) J. Fish Dis. 8 , 289–298.  (3) Chan, D., Tarbin, J.A., Stubbings, G., Kay, J., & Sharman, M. (2012 ) Food Addit. Contam. A 29 , 66–72.  (4) Wan, H., Weng, S., Liang, L., Lu, Q., & He, J. (2011) Food Chem. Toxicol . 49 , 3031–3037.  (5) Culp, S.J., Mellick, P.W., Trotter, R.W., Greenlees, K.J., Kodell, R.L., & Beland, F.A. (2006) Food Chem. Toxicol . 44 , 1204–1212.  (6) Srivastava, S., Sinha, R., & Roy, D. (2004) Aquatic Toxicol . 66 , 319–329.  (7)  Official Methods of Analysis (2012) 19th Ed., Standard Method Performance Requirements for Quantitative Methods for Drug Residues in Shrimp, Tilapia, Catfish, and Salmon , AOAC INTERNATIONAL, Rockville, MD, SMPR 2009.001 , approved by the AOAC Stakeholder Panel on Marine and Freshwater Foods (SPMFF) 3/31/2010  (8) Hurtaud-Pessel, D., Couëdor, P., & Verdon, E. (2013) J. AOAC Int. 96 , 1152–1157.  (9) U.S. Food and Drug Administration (2012) Guidelines for the Validation of Chemical Methods for the FDA Foods Program Version 1.0, Office of Foods and Veterinary Medicine. http:// UCM298730.pdf (10) Commission Decision 2002/657/EC (12 August 2002) Off. J. Eur. Commun. L221 , 8–36 (11)  Guidance for Industry: Mass Spectrometry for Confirmation of the Identity of Animal Drug Residues (2003) Guidance 118, U.S. Food and Drug Administration, Center for Veterinary Medicine, Fed. Regist . 68 , 25617–25618. AnimalVeterinary/ GuidanceComplianceEnforcement/ GuidanceforIndustry/ucm052658.pdf (12) Hurtaud-Pessel, D., Couëdor, P., & Verdon, E. (2011) J. Chromatogr. A 1218 , 1632–1645. (13) Andersen, W.C., Turnipseed, S.B., Karbiwnyk, C.M., Lee, R.H., Clark, S.B., Rowe, W.D., Madson, M.R., & References


This method has provided clearly acceptable results at and below the level of interest (1 µg/kg) for the triphenylmethane dyes studied. The method accuracy was excellent with trueness generally ≥90%, precision generally ≤10% RSDr, and HorRat values <1. The Study Directors recommend this method for acceptance as Final Action status.


We thank John Phillips (U.S. Department of Agriculture, Agricultural Research Service, Wyndmoor, PA) for performing the statistical analysis for this study. We also acknowledge the following individuals from the FDA for their technical assistance with the preparation of the study samples: Sherri Turnipseed and Joseph Storey (Animal Drugs Research Center, Office of Regulatory Affairs, Denver Laboratory, Denver, CO); Christine Casey, Edward Iannuzzi, Ryan Stadtmuller, Julie Lillehaugen, Andrea Heise, Zachary Miller, Ashleigh Gillaspie, and Mark Madson (Office of Regulatory Affairs, Denver Laboratory, Denver, CO); and Eric Evans and Scott Frobish (Center for Veterinary Medicine Aquaculture Program, Laurel, MD). We thank Sherri Turnipseed and Steve Lehotay (USDA- ARS, Wyndmoor, PA) for assistance with design of the study protocol, Kai Klocke for assistance with programming and data transformation, and Tom Phillips (Maryland Department of Agriculture, Annapolis, MD) for additional statistical review. Finally, we acknowledge the following collaborators for their participation in this study: Mark Crosswhite and Walter Hammack, Florida Department of Agriculture and Consumer Services, Division of Food Safety, Chemical Residue Laboratory, Tallahassee, FL Christopher K. Lam and Mary Cumming, Tennessee Department of Agriculture, Ivy Laboratory, Nashville, TN Sarah R. Ruiz and Cheryl D. Stephenson, Eurofins Central Analytical Laboratories, New Orleans, LA Alan R. Lightfield and Steven J. Lehotay, U.S. Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, Wyndmoor, PA Dominique Hurtaud-Pessel, Pierrick Couëdor, and Eric Verdon, ANSES, French Agency for Food, Environmental and Occupational Health Safety, Laboratory of Fougères, EU-RL for Antibiotic and Dye Residues, Fougères, France Mike Filigenzi and Robyn Noonan, California Animal Health and Food Safety Laboratory, University of California at Davis, Davis, CA

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