OMA Protocol Review: OMAMAN-56 Sulfites in Shrimp

Biolan Microbiosensores BIOFISH 300 SUL Collaborative Study Protocol

February 2019

independently and all laboratories will preferably be in the EU for ease of shipping samples and equipment. An effort will be made to recruit both government and private laboratories. In addition, 3 collaborators will be recruited for the OMA method, but these may be collaborators that are not performing the Biofish method. A sample letter to collaborators can be found in Appendix 3.1. This letter will be sent to each collaborator prior to the start of the study. In addition, a conference call will be held with collaborators to review the study protocol in detail and answer any questions before the start of the study. 2.3 Collaborative Study Design 2.3.1 The study will include 6-12 test sites, with no more than 2 collaborators at any one site. The 2 collaborators may be 2 analysts employed at that site but working independently. 2.3.2 Six materials will be analyzed in the collaborative study. A material is an analyte/matrix/concentration combination. The materials will all be incurred samples sourced from seafood producers. Two materials will be used to test each method range. The low range, 7-30 mg/kg, is validated only for boiled shrimp and raw shrimp with heads off. Boiled shrimp tend to have the lowest sulfite levels and shrimp with heads on tend to have the highest sulfite levels due to the fat content in the heads. The proposed Study Materials in Table 1 take these facts into account. 2.3.3 Collaborators will each receive 2 replicate test portions of each material for a total of 12 test portions as described in Table 1. All test portions for each collaborator will be randomized and blind coded. The randomization will be different for each collaborator. A test portion inventory sheet will be shipped with each test portion set to verify receipt of correct test portions and to indicate which blind coded test portions to use for which method range. 2.3.4 In addition, three collaborators will analyze 2 replicates of each material by the OMA 990.28 reference method. Table 1. Test portion set for each collaborator Material* Test Portion Size Number of Test Portions Method Range No. Matrix Sulfite Concentration 1 Boiled shrimp 7-12 mg/kg 2 g 2 7-30 mg/kg 2 100-150 mg/kg 2 g 2 50-300 mg/kg 3 Raw shrimp with heads off 15-20 mg/kg 2 g 2 7-30 mg/kg 4 40-50 mg/kg 2 g 2 30-150 mg/kg 5 Raw shrimp with heads on 80-100 mg/kg 2 g 2 30-150 mg/kg 6 250-300 mg/kg 2 g 2 50-300 mg/kg *All materials are incurred matrix.

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DRAFT