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 Varies depending on the analyte. Generally, low is from 2 ppb to 25 ppb. High is 20 ppb to 250 ppb. ER 2 Range varies and is dependent on the specific analyte. This is appropriate as lower molecular weight PAHs are generally found in higher concentrations than higher molecular weight PAHs. It is acceptable for this application as levels of concern for low molecular weight PAHs are significantly higher. ER 3 Sufficient. ER 4 BaP: 0.5 - 100 μg/kg (0.5, 1, 2, 5, 10, 20, 50, 100) Other PAHs: 1.25 - 250 μg/kg (1.25, 2.5, 5, 12.5, 25, 50, 125, 250) naphthalene: 2.5 - 500 μg/kg (2.5, 5, 10, 25, 50, 100, 250, 500) ER 5 Good ER 6 Suitable ER 7 0.5 to 100 ug/kg for BaP and other lower-level PAHs; 1.25 to 250 ug/kg for higher-level PAHs; and 2.5 to 500 ug/g for naphthalene. ER 8 good ER 2 LOQ varies and is dependent on the specific analyte. This is appropriate as lower molecular weight PAHs are generally found in higher concentrations than higher molecular weight PAHs. It is acceptable for this application as levels of concern for low molecular weight PAHs are significantly higher. ER 3 Please see comment above about spike levels and LOQ of BaP. ER 4 Bap: 0.5 μg/kg Other PAHs: 1.25 μg/kg naphthalene: 2.5 μg/kg ER 5 Good ER 6 Suitable ER 7 1 ug/kg for BaP and other lower-level PAHs; 2.5 ug/g for higher-level PAHs; and 5 ug/g for naphtalene. ER 8 good LOQ ER 1 Not discussed in the method. Likely in the low ppbs. Analytical Range

Accuracy/Recovery

ER 1 ER 2 ER 3

Varies depending on the analyte. 70-120% mostly. Accuracy/Recovery is high and meets validation criteria.

Good

ER 4 In shrimp: 83.8-115% In mussel: 77.3-107% In oyster: 71.6-94.6%, except for a lower mean recovery of 68.6% for benzo[α]anthracene (BaA) in oyster, and 50.3-56.5% and 48.2-49.7% for anthracene and beno[α]pyrene, respectively. ER 5 Good ER 6 As noted by the authors, the recoveries for the oyster tissue are low and probably inadequate. ER 7 After excluding the outliers, the mean recoveries (8-10 labs) are in the range of 70-120% with a few exceptions which may due to the compound degradation in oyster samples stored at -20 C. ER 8 good