AOAC-RI ERP Book - FAOM METHOD.pdf

AOAC RESEARCH INSTITUTE AOAC OFFICIAL METHODS OF ANALYSIS (OMA) OMAMAN-15 : Determination Of Polycyclic Aromatic Hydrocarbons (PAHs) In Seafood Using Gas Chromatography-Mass Spectrometry: A Collaborative Study* Study Director: Katerina Mastovska, Covance Laboratories Inc., Nutritional Chemistry and Food safety, 3301 Kinsman Boulevard, Madison, WI 53704, USA ER 1 This study successfully addressed the urgent need for a reliable approach to analyzing various PAHs in potentially contaminated seafood’s. Method procedures are easy to follow and not time-consuming. ER 2 The validation procedure outlined in this document was comprehensive and the results demonstrated that the method was accurate and rugged. This method is a significant improvement over current regulatory methods. It is significantly faster, requires less organic solvent and produces less waste, less labor intensive and is easier to perform that the current method, while fulfilling required method performance benchmarks. ER 3 none ER 4 The collaborative study report was a very clear presentation. The experiment or study was thorough and well designed. Performance-based criteria led to a robust method for analysis of PAHs in seafood. The method was practical and fit for purpose. Results from collaborative study supported the method performance and demonstrated that the method was fit- for-purpose to determine PAHs and their alkyl homologues in seafood. ER 5 Method is well-written but needs more specificity in select sections. For example, on page 6, under (5), it is stated all analytes of reagent blanks must be below the concentrations in the lowest calibration standard. Needs more clarification....how far below? Also, since stability of some PAHs was questionable, a Stability Study needs to be carried out with PAH standards stored at varying temperatures and times. The Safety Section must be in the front of the method since safety is more important than any other part of the protocol. ER 6 None ER 7 The method is quick, easy to use, and allows flexibility in method development. It demonstrated good GC separations of isomer pairs, excellent recoveries and reproducibility were achieved except for 2 compounds in oyster which might degrade at -20 C, no degradation was observed when oyster was stored at -70 C, however it's not very practical for many labs to maintain such low storing temperature. ER 8 Very good method ER 2 The method is well written and easily understood. The instructions are clear and I found no ambiguities. ER 3 The method as written is clean with only a few instances for improvement. Performance criteria and how to evaluate the criteria are nicely described. ER 4 The method procedure is well described and steps are easy to follow. ER 5 Method is generally clear but needs more specificity in select areas. ER 6 The method is clear and all the necessary information provided to reproduce and use the method. The authors should use correct nomenclature for the PAHs, i.e., Benzo[ghi]perylene not benzo[g,h,i]perylene ER 7 The method is clearly described in the manuscript. ER 8 good Method Clarity ER 1 Good clarity throughout the manuscript. General Comments