QuPPe-AO - EURL | Residues of Pesticides

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3.11. Pesticide stock solutions, See latest version of QuPPe-PO-Method. Use plastic flasks and stoppers if pesticides that tend to interact with glass-surfaces are present (e.g. Glyphosate, Ethephon). 3.12. Pesticide working solutions / mixtures, See latest version of QuPPe-PO-Method. Use plastic flasks and stoppers if pesticides that tend to interact with glass-surfaces are present (e.g. Glyphosate, Ethephon). 3.13. Internal Standards (ISTDs), See latest version of QuPPe-PO-Method. 3.14. ISTD Stock solutions, See latest version of QuPPe-PO-Method. Use plastic flasks and stoppers if pesticides that tend to interact with glass-surfaces are present (e.g. isotope labeled Glyphosate, Ethephon). 3.15. ISTD-working solution I (ISTD-WS I) for spiking samples prior to extraction, See latest version of QuPPe-PO-Method. Use plastic flasks and stoppers if pesticides that tend to interact with glass-surfaces are present (e.g. isotope labeled Glyphosate, Ethephon). 3.16. ISTD-working solution II (ISTD-WS II) for preparation of calibration standards, See latest version of QuPPe-PO-Method. Use plastic flasks and stoppers if pesticides that tend to interact with glass-surfaces are present (e.g. isotope labeled Glyphosate, Ethephon). 4. Disclaimer This method refers to several trade name products and instruments which are commercially available and suitable for the described procedure. This information is given for the convenience of the users of this method and does not constitute an endorsement by the EURL of the products named. The application of this method may involve hazardous materials, operations and equipment. It is the responsibility of the users of this method to establish appropriate safety and health practices prior to use. EU Reference Laboratory for pesticides requiring Single Residue Methods (EURL-SRM) CVUA Stuttgart, Schaflandstr. 3/2, DE-70736 Fellbach, Germany Website: www.eurl-pesticides.eu, E-Mail: EURL@cvuas.bwl.de 4 of 15
5. Procedure 5.1. Sample preparation To obtain representative test-portions from the laboratory sample, proceed as required by the respective regulations and guidelines. Homogenize the eggs with a hand-blender (2.1) until a free flowing mixture is obtained. Proceed similarly with non-homogenized milk (e.g. if fat has separated). 5.2. Extraction / Centrifugation / Filtration 5.2.1. Weigh a representative portion (ma) of the sample homogenate (5.1) into a 50 mL centrifuge tube (2.2). In case of fresh milk and fresh eggs take 10 g 0.05 g of the homogenized sample. 5.2.2. Add water (3.1) to a content of ca. 10 g in total. In the case of cow milk (88 % water) add 1.2 g of water and in case of chicken eggs (76% water) add 2.4 g of water. Notes: - Where no IL-ISTDs are used or where they are added after extract aliquotation, water adjustment is essential. Where the appropriate IL-ISTDs are employed before any aliquotation has taken place water adjustment is less critical and can be skipped for commodities containing ≥80% water. 5.2.3. Add 10 mL acidified methanol (3.6) and 50 µL of the ISTD-WS I (3.15) containing isotopically labeled analogues of one or more of the analytes of interest (added ISTD mass = mISTD sample ). Notes: - For screening purposes the ISTD can be alternatively added to an aliquot of the final sample extract (see 5.2.10) 5.2.4. Close the tube and shake vigorously for 1 min by hand or for 5-20 minutes by a mechanical shaker. 5.2.5. Centrifuge for 5 min at >3000 g. 5.2.6.Transfer a 2 mL aliquot into a 10 mL centrifuge tube with screw cap (2.3), which already contains the 2 mL of acetonitrile (3.3) and 100 mg of ODS sorbent (3.7). 5.2.7. Close the tube and shake vigorously for 1 min by hand. 5.2.8. Centrifuge (e.g. for 5 min at >3000 g). 5.2.9.Filter an aliquot (ca. 3-4 mL) of the extract through a syringe filter (2.7) into a sealable storage ves- sel. 5.2.10. Transfer, as required, one or more aliquots (e.g. 1 mL each) into auto-sampler vials (2.9) Notes: - The cleaned-up extract will contain ca. 0.25 g sample equivalents per mL extract (if 10 g sample are employed for extraction). - Instead of adding the ISTD at the beginning of the procedure it can be added to an aliquot (e.g. 1 mL) of the final sample extract. This way the added amount of ISTD per sample can be drastically reduced (e.g. 40-fold if added to 1 mL extract). The ISTD added at this step will compensate for ma- EU Reference Laboratory for pesticides requiring Single Residue Methods (EURL-SRM) CVUA Stuttgart, Schaflandstr. 3/2, DE-70736 Fellbach, Germany Website: www.eurl-pesticides.eu, E-Mail: EURL@cvuas.bwl.de 5 of 15
Page 1 and 2: Quick Method for the Analysis of Re
Page 3: 2.10. Volumetric flask with stopper
Page 7 and 8: Table 1: Exemplary pipetting scheme
Page 9 and 10: 5.6. LC-MS/MS Measurement Condition
Page 11 and 12: Figure 5: Chromatograms of Trimethy
Page 13 and 14: 5.7.2.2. Calculations when employin
Page 15: Table 5: Document History Action Wh

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