Reaktion #1761652

ord-dfd52f1b4a04492c84128af2e0151717

Reagenzien

Keine

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwere added to extracts
  2. 2
    Sonstigeto ion exchange SPE purification
  3. 3
    SonstigeFinal extracts were prepared in aqueous 0.02M phosphoric acid
  4. 4
    Filtrationfiltered (0.2 μm)
  5. 5
    Sonstigeto LC/MS/MS analysis to remove particulates as preventive maintenance measure for the HPLC system

Vorschrift

Glyphosate and/or AMPA stable isotope standards used as internal standards were added to extracts prior to ion exchange SPE purification. Final extracts were prepared in aqueous 0.02M phosphoric acid and filtered (0.2 μm) prior to LC/MS/MS analysis to remove particulates as preventive maintenance measure for the HPLC system. Phosphoric acid acts a weak ion-pairing agent on HPLC polymeric stationery phase and was used as the final solution to improve glyphosate LC/MS/MS performance (response and linearity). The analytes were resolved by HPLC reverse-phase chromatography using a phenyl-hexyl column coupled to electrospray ionization in with MS/MS detection to acquire 2 molecular ion transitions (only 1 ion transition is monitored for AMPA in positive ion mode). Quantitative analysis was accomplished using a single molecular ion transition. The relative abundance of the 2 MS/MS fragment ions provided confirmatory evidence for glyphosate, N-acetylglyphosate, N-acetyl AMPA, and AMPA (negative mode).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08003398B2uspto-grants-2011_08