sign in sign up
<<
Home , Cefapirin, Flugestone acetate

AOAC SMPR® 2018.010 Probability of detection (POD).—Proportion of positive analytical outcomes for a qualitative method for a given matrix at a given analyte level or concentration. [Appendix H: Probability Standard Method Performance Requirements (SMPRs®) for Screening and Identification Method of Detection (POD) as a Statistical Model for the Validation for Regulated Veterinary Drug Residues in Food of Qualitative Methods, Official Methods of Analysis of AOAC INTERNATIONAL (2019) 21st Ed., AOAC INTERNATIONAL, Intended Use: Routine Surveillance for GMP Compliance Rockville, MD, USA (http://www.eoma.aoac.org/app_h.pdf)] 5 Method Performance Requirements 1 Purpose See Table 2. AOAC SMPRs describe the minimum recommended performance characteristics to be used during the evaluation of a 6 System Suitability Tests and/or Analytical Quality Control method. The evaluation may be an on-site verification, a single- Suitable methods will include blank check samples and check laboratory validation, or a multi-site collaborative study. SMPRs standards at 0.5x MRL prepared in matrix. Method developers will are written and adopted by AOAC stakeholder panels composed of provide information on how cutoffs are determined. representatives from the industry, regulatory organizations, contract 7 Reference Material(s) laboratories, test kit manufacturers, and academic institutions. AOAC SMPRs are used by AOAC expert review panels in their Refer to Annex F: Development and Use of In-House Reference evaluation of validation study data for method being considered Materials in Appendix F: Guidelines for Standard Method for Performance Tested MethodsSM or AOAC Official Methods of Performance Requirements, 21st Ed. of the Official Methods of AnalysisSM, and can be used as acceptance criteria for verification Analysis of AOAC INTERNATIONAL (2019). Available at http:// www.eoma.aoac.org/app_f.pdf at user laboratories. 2 Applicability 8 Validation Guidance

A method or a suite of methods that can screen for and identify Appendix D: Guidelines for Collaborative Study Procedures to regulated veterinary drug residues with established maximum Validate Characteristics of a Method of Analysis, 21st Ed. of the residue limits (MRLs) in bovine milk, muscle, and fat; chicken Official Methods of Analysis of AOAC INTERNATIONAL (2019). muscle, skin with adhering fat, and eggs; and fish. Table 1 is provided Available at http://www.eoma.aoac.org/app_d.pdf as guidance on veterinary drug residue/matrix combinations and Appendix F: Guidelines for Standard Method Performance associated MRLs. Additional matrices may be added as appendices Requirements, 21st Ed. of the Official Methods of Analysis of to this SMPR in the future. A single method is not required to cover AOAC INTERNATIONAL (2019). Available at http://www.eoma. all drug/matrix combinations, but method developers should strive aoac.org/app_f.pdf to include as many relevant drug residues as possible for each Method developers may prepare cocktails of multiple drug matrix claimed. Method developers may choose to claim one or residues. Method developers are cautioned that some drug residues more matrices. may have additive or masking effects when combined and should be prepared to demonstrate that these concerns have been addressed 3 Analytical Technique with their submitted materials/data. Method developers should Liquid chromatography-tandem mass spectrometry (LC-MS/ consider the stability of drug residues in cocktails and be prepared MS), using low- or high-resolution MS. to demonstrate that these concerns have been addressed in their 4 Definitions data submission package. Maximum residue limit (MRL).—The maximum allowable Performance criteria in Table 2 are for single-laboratory concentration of a drug residue in a particular matrix. Also known validation. Method developers should contact AOAC for as “tolerance” in the United States. MRL varies by matrix and by developing a collaborative study design. country or regulatory agency. For the purposes of this SMPR, the Method developers must provide the precursor ion and at least lowest MRL currently in effect amongst European Union (EU), two standard reference material (SRM) transitions with ion ratios Codex, Canada, China, and U.S. regulations will be used as “the and retention parameters for each veterinary drug. MRL.” In cases in which an MRL applies to the sum of metabolites 9 Maximum Time-to-Result or sum of drugs, that MRL was chosen over MRLs for a single None metabolite or marker residue. If no MRL is provided in Table 1 (shaded cells), then the drug is either prohibited in that matrix by Approved by the AOAC Stakeholder Panel on Strategic Food one or more regulatory agencies or an MRL is not required. Analytical Methods (SPSFAM). Final Version Date: August 26, 2018.

© 2018 AOAC INTERNATIONAL 500 200 4000 Raw whole chicken egg 50 50 12 Raw fish 40 10 10 50 50 50 500 500 100 200 skin/fat Raw chicken a 40 10 10 50 50 50 500 500 100 200 muscle Raw chicken Lowest global MRL, μg/kg 5 10 10 10 50 50 50 100 200 500 200 0.75 2000 1000 Raw bovine fat 5 10 10 10 50 50 100 500 500 200 500 200 0.75 muscle Raw bovine b 4 4 1 10 30 20 60 50 0.3 0.1 100 100 125 100 milk Liquid bovine

moiety Cefapirin Carprofen Deacetylcefapirin Regulated marker Albendazole oxide Albendazole sulfone Albendazole sulfone Albendazole sulfoxide Carprofen glucuronide Dichloroisoeverninic acid Albendazole 2-aminosulfone Albendazole 2-aminosulfone Sum of metabolites containing 2,4-DMA Sum of metabolites containing 2,4-DMA Veterinary drugs residues in bovine milk, muscle, fat, chicken skin/fat, fish, and eggs Veterinary 1. Table Compound Abamectin (B1a) Acetylisovaleryltylosin Albendazole Albendazole Albendazole Albendazole Oxide Albendazole Oxide Albendazole Oxide Amitraz Amprolium Apramycin Avilamycin (A, B, C) Baquiloprim Bicozamycin Buquinolate Cabergoline Carazolol Carprofen Carprofen Cefacetril Cefapirin Cefapirin

© 2018 AOAC INTERNATIONAL 30 50 400 300 300 Raw whole chicken egg 50 10 900 200 300 150 100 Raw fish 1 50 50 50 200 300 150 100 500 5000 2000 1000 skin/fat Raw chicken 1 30 50 50 200 300 150 100 200 500 5000 1000 muscle Raw chicken Lowest global MRL, μg/kg 4 1 1 50 20 10 50 50 50 0.2 200 100 200 150 400 200 100 700 2000 3000 2000 Raw bovine fat 5 50 20 35 10 10 20 20 70 10 20 50 0.1 200 100 200 150 0.75 1000 1000 1000 muscle Raw bovine 50 20 20 16 45 10 50 20 30 20 30 20 20 2.5 0.3 0.1 100 100 200 milk 0.05 Liquid bovine c c

Ceftiofur Cypermethrin Chlortetracycline Desfuroylceftiofur Regulated marker Alpha-Cypermethrin 4-epi-chlrotetracycline Para-toluenesulfonamide ) continued ( 1. Table Compound Ceftiofur Chloramine-T Chlortetracycline Chlortetracycline Clenbuterol Clopidol Clorsulon Closantel Cyfluthrin Cyhalothrin Cypermethrin Cypermethrin Cyromazine Danofloxacin Decoquinate Deltamethrin Diaveridine Diazinon Dichlorvos Diclazuril Diclofenac

© 2018 AOAC INTERNATIONAL 25 20 400 Raw whole chicken egg 10 50 300 300 500 100 100 200 500 1000 Raw fish 30 40 30 50 300 400 600 300 100 100 200 250 skin/fat Raw chicken 30 30 50 300 300 600 100 100 100 500 100 400 muscle Raw chicken Lowest global MRL, μg/kg 50 10 20 300 100 600 150 300 100 150 100 100 250 200 300 7000 Raw bovine fat 10 50 50 25 20 300 400 600 500 100 100 100 100 200 200 200 muscle Raw bovine 1 30 15 12 10 40 10 50 200 150 100 milk Liquid bovine

Florfenicol Doxycycline Enrofloxacin Ciprofloxacin Flubendazole Fenbendazole Florfenicol-amine Regulated marker Eprinomectin (B1a) Oxfendazole sulphone Oxfendazole sulphone Fenbendazole Sulfoxide fluorophenyl)methanone 2-amino 1H-benzimidazol-5-yl-(4- Sum of dihydrostreptomycin + streptomycin ) d inued t con ( 1. Table Compound Difloxacin Dihydrostreptomycin Diminazene Doramectin (B1a) Doxycycline Emamectin (B1a) Enramycin Enrofloxacin Enrofloxacin Eprinomectin Erythromycin Ethopabate Eugenol Famphur Febantel Fenbendazole/ Oxfendazole Fenbendazole/ Oxfendazole Fenbendazole Fenvalerate Flavophospholipol Florfenicol Florfenicol Fluazuron Flubendazole Flubendazole Flumequine

© 2018 AOAC INTERNATIONAL 50 50 200 1300 Raw whole chicken egg 10 50 50 500 100 6000 1350 Raw fish 20 40 40 10 50 75 100 100 100 200 100 100 skin/fat Raw chicken 10 40 20 10 100 100 200 100 100 muscle Raw chicken Lowest global MRL, μg/kg 5 30 20 50 20 50 40 10 50 50 20 10 150 100 100 100 100 Raw bovine fat 1 10 20 20 50 10 10 50 10 20 20 10 100 300 100 100 250 100 150 100 muscle Raw bovine 2 2 30 10 50 50 75 15 50 100 100 150 150 milk Liquid bovine

Flunixin Ivermectin B1a 5-hydroxyflunixin Regulated marker 4-Methylaminoantipyrin Sum of C1, C1a, C2, C2a ) continued ( 1. Table Compound Flumethrin Flunixin Flunixin Fluralaner Fluvalinate Gamithromycin Gentamicin(s) Halofuginone Haloxon Hexaflumuron Imidocarb Isoeugenol Isometamidium Ivermectin Josamycin Kanamycin A Ketoprofen Kitasamycin Lasalocid A Levamisole Lincomycin Lufénurone Maduramicin Marbofloxacin Mebendazole acetate Meloxicam Metamizol

© 2018 AOAC INTERNATIONAL 500 400 Raw whole chicken egg 50 50 500 100 300 200 500 Raw fish 20 50 50 30 20 50 50 50 500 100 100 200 150 100 300 200 1000 skin/fat Raw chicken 20 10 15 30 20 500 100 100 200 150 100 300 100 200 500 1000 muscle Raw chicken Lowest global MRL, μg/kg 10 50 20 50 20 50 50 0.2 100 500 300 500 200 150 300 100 200 1000 Raw bovine fat 2 20 15 20 20 50 50 0.2 100 300 500 400 150 300 100 100 200 500 1000 muscle Raw bovine 2 50 40 30 50 50 20 30 50 10 150 100 100 milk 0.12 Liquid bovine c c

Penicillin G G Neomycin B Oxytetracycline Regulated marker Albendazole oxide Albendazole sulfone 4-epi-oxytetracycline Albendazole 2-aminosulfone N-methyl-1,3-propanediamine ) continued ( 1. Table Compound Metoserpate Monensin Morentel Moxidectin Narasin Neomycin Nequinate Netobimin Netobimin Netobimin Nicarbazin Nitroxinil Nosiheptide Novobiocin Oleandomycin Orbifloxacin Ormetoprim Oxibendazole Oxolinic acid Oxyclozanide Oxytetracycline Oxytetracycline Paromomycin Penethamate Penicillin G ()

© 2018 AOAC INTERNATIONAL 25 60 20 0.7 100 500 400 2000 1000 Raw whole chicken egg 10 300 200 100 300 200 Raw fish 25 50 10 0.7 550 100 200 100 500 100 300 600 100 200 skin/fat Raw chicken 25 25 50 10 50 0.7 100 500 100 500 100 100 200 600 100 200 muscle Raw chicken Lowest global MRL, μg/kg 4 50 10 30 50 500 400 100 500 500 300 600 100 100 Raw bovine fat 4 50 50 50 10 30 50 100 100 500 250 200 600 100 100 muscle Raw bovine 6 50 50 50 10 60 100 200 200 200 100 100 milk Liquid bovine c c

Arsenic Pyrantel Spiramycin Tetracycline Neo-Spiramycin 4-epi-tetracycline Regulated marker sulfonamide group N-methyl-1,3-propanediamine Sum of all substances belonging to the Sum of dihydrostreptomycin + streptomycin )

d continued ( 1. Table Compound Penicillin V () Permethrin Phoxim Piperazine Piperonyl butoxide Pirlimicyn Pyrantel Pyrantel Pyrimethamine Ractopamine Rafoxanide Rifaximin Robenidine Roxarsone (Arsanilic acid) Salinomycin Sarafloxacin Semduramicin Spectinomycin Spiramycin Spiramycin Streptomycin Sulfonamide Teflubenzuron Tetracycline Tetracycline

© 2018 AOAC INTERNATIONAL 200 200 1000 Raw whole chicken egg 50 50 10 10 50 100 Raw fish 50 75 50 50 100 200 100 400 2000 skin/fat Raw chicken 50 75 50 100 100 100 100 3000 muscle Raw chicken Lowest global MRL, μg/kg 50 50 50 50 50 100 150 100 200 100 100 1000 Raw bovine fat 2 2 2 50 50 50 50 50 100 400 100 200 200 100 100 muscle Raw bovine 50 50 50 50 50 10 50 20 50 milk Liquid bovine

Zoalene Tiamulin Tylvalosin Thiabendazole Beta- 3-O-acetyltylosin Toltrazuril sulfone Toltrazuril Regulated marker Ketotriclabendazole 8-alpha-hydroxymutilin 5-hydroxy-thiabendazole 3-amino-5-nitro-o-toluamide ) continued ( Method developers should verify the definition of marker residue. applies to the sum of dihydrostreptomycin and streptomycin. MRL MRL applies to the sum of chlortetracycline, oxytetracyclin, tetracycline, and their epimers. MRL Shaded cells = If no MRL is provided, then the drug is either prohibited in that matrix by one or more regulatory agencies or an MRL is not required. is provided, then the drug either prohibited in that matrix by one or more regulatory agencies an MRL Shaded cells = If no MRL   

1. Table Compound Thiabendazole Thiabendazole Thiamphenicol Tiamulin Tiamulin Tildipirosine Tilmicosin acid Tolfenamic Toltrazuril Trenbolone methanesulfonate Tricaine Trichlorfon Triclabendazole Trimethoprim Tripelennamine A Tulathromycin Tylosin Tylvalosin Tylvalosin (M1) Virginiamycin Zeranol Zilpaterol Zoalene (Dinitolmide) Zoalene (Dinitolmide) a b c d

© 2018 AOAC INTERNATIONAL Table 2. Method performance requirements Residue concn in matrix N Acceptance criterion 0 (Blank) 30 ≤10% POD with 95% confidence 0.5x MRL 30 per druga ≥90% POD with 95% confidenceb a Tested as drug cocktail(s). b All incorrect results must be investigated for determination of

concentration at which POD90 with 95% confidence is achieved.

© 2018 AOAC INTERNATIONAL