OMA Protocol Review: OMAMAN-56 Sulfites in Shrimp

Biolan Microbiosensores BIOFISH 300 SUL Collaborative Study Protocol

February 2019

KITMFSUL/SEFSUL: According to Regulation (EC) No. 1272/2008:

Hazard Statements : H319. Eye Irrit.2. May cause serious eye irritation. Precautionary Statements :

P264 Wash thoroughly after handling. P280 Wear eye protection/face protection. P305+P351+P338 In case of eye contact: rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. P337+P313 If eye irritation persists, get medical advice. Test Portion Analysis On Wednesday, all collaborators shall initiate the extraction and analysis of test portions according to the BIOFISH 300 SUL method (Appendix 3.3). A copy of the detailed method will be provided for you. It is important that all collaborators perform the study on the same day and complete all the testing within one day. All test portions are pre-weighed. Each collaborator will analyze their test portions as follows. 1. Refer to the Test Portion Inventory Sheet for the BIOFISH 300 SUL range to use for each test portion. There are 4 blind coded test portions for each method range. Group the test portions by range keeping them frozen. 2. Starting with the test portions for the first range, for example, 7-30 mg/kg, allow the appropriate test portions to sit at room temperature for no more than 15 minutes to thaw, with the plastic tube closed, as it was received. 3. Add 18 mL of SUL extraction solution. 4. Homogenize the contents with the aid of an UltraTurrax set at 8000-9000 rpm for 15-20 sec. 5. Let stand a minimum of 15 minutes at room temperature to complete the extraction. Once extracted, the samples are stable up to 1 h at room temperature. 6. Follow the BIOFISH 300 SUL 7-30 mg/kg method to set up the device (recondition, activation and calibration). 7. Follow the BIOFISH 300 SUL 7-30 mg/kg method to complete the analyses. 8. Repeat steps 2 –7 for the other two method ranges. 9. Record all results on the Data Report Form (Appendix 3.5). Select collaborators, as prearranged, will receive a set of 6 blind coded test portions for the OMA 990.28 method. Analyze these test portions also beginning on Wednesday as follows. Keep each test portion 2. Thaw each test portion just prior to analysis. 3. Add 100 mL 5% EtOH in water v/v and blend. 4. Transfer test suspension to prepared apparatus. 5. Allow all but 2-3 mL of HCl solution from separatory funnel to drip into flask containing test suspension. 6. Boil contents of flask for 1.7 h. frozen until ready for analysis. Complete the OMA analyses within 3 days. 1. Prepare apparatus and solutions according to the OMA 990.28 method.

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DRAFT