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Application of HR-LC-MS in screening methods for pesticides in cereals

Application of HR-LC-MS in screening methods for pesticides in cereals. Anne Kruse Lykkeberg, Mette Erecius Poulsen Almeria, 12 June 2014. Disposition. LC-QTOF instruments. Disposition. PCD – CSV file. QTOF-analysis – MS scan. Used to determine retention time. No selection.

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Application of HR-LC-MS in screening methods for pesticides in cereals

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  1. Application of HR-LC-MS in screening methods for pesticides in cereals Anne Kruse Lykkeberg, Mette Erecius Poulsen Almeria, 12 June 2014

  2. Disposition

  3. LC-QTOF instruments

  4. Disposition

  5. PCD – CSV file

  6. QTOF-analysis – MS scan • Used to determine retention time No selection No collision

  7. PCDL - library

  8. PCDL – library - spectra

  9. QTOF-analysis – Targeted MS/MS • Obtaining compound spectra for Library • Spectra of daughter ions from the single ion isolated in the quadropole Selection of single mass Collision 10, 20 and 40 V

  10. QTOF-analysis – All ion MS • MS scan with collision energy • Screening samples • Spectra of daughter ions of all compounds eluting on a certain time point No selection Collision 10, 20 and 40 V

  11. Chromatogram - TIC

  12. Spectra – MSscan incl. collision Ofurace, [M+H]+ 0V 10V 20V 40V

  13. Disposition

  14. Standard mixtures

  15. Spectra of isomers in Agilents library Prometon Terbumeton Secbumeton

  16. Disposition

  17. Validation • My alternative validation plan • 20-25 samples – spiked at 0.1 mg/kg • 10-20 blank samples

  18. Dilution of spiked samples Spiked rye is diluted with Blank rye … Matrix is the same Recovery is assumed to be the same at the different concentration levels

  19. Disposition

  20. Compound list – exported to Excel

  21. All file gathered in one Excel-file

  22. Area of all samples spiked at 10 ppb

  23. Comparison of areas in spiked samples with blank

  24. Disposition

  25. Virtual computers for data-analysis Challenges • The Agilent software demands Windows Professional 64 bit – englishversion • Back up of all laboratory computer on LAB-domain • Laboratory domain, with no access from personal computers Solution • Virtual computers from Citrix • On the Laboratory domain • Windows Professional 64 bit • Access to all data – back up early in the morning • Few licenses are necessary • Access from all computers with internet

  26. Disposition

  27. FVII cocktail IV – project • Aim is to develop a cereal-method to analyze many analytes in one method. • Analytes: • Pesticides (The pesticides most present in cereal – in practice the standard mixtures which we use for our quantitative methods). • Mycotoxins: Most important mycotoxins in cereals.

  28. Method development - QuEChERS

  29. Extraction

  30. Phase separation

  31. Freeze out step

  32. PSA clean up

  33. Analytes Add Presentation Title in Footer via ”Insert”; ”Header & Footer”

  34. Extraction

  35. Phase separation

  36. Freeze out step

  37. PSA clean up

  38. Analytes

  39. TIC af blank ipositiv mode

  40. TIC af blank ipositiv mode

  41. TIC af blank inegativmode

  42. TIC af blank inegativmode

  43. Matrix effect & recovery – Mycophenol acid • Mycophenol acid • 6.63 min • Mass: 320.1260

  44. Matrix effect & recovery – Fumonisin B2 • Fumonisin B2 • 5.07 min • Mass: 705.3936

  45. Matrix effect & recovery – Roquefortin C • Roquefortin C • 5.15 min • Mass: 389.1852

  46. Matrix effect & recovery – Clothianidin • Clothianidin • 4.46 min • Mass: 249.0087

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