alpha-AMINO-3-HYDROXY-5-METHYL-4-ISOXAZOLEPROPIONIC ACID → alpha-AMINO-3-HYDROXY-5-METHYL-4-ISOXAZOLEPROPIONIC ACID

HRID 1674470

反応式

HRID 1674470 の反応式
[CH2:1]([NH:5][CH2:6][P:7]([OH:10])([OH:9])=[O:8])[C:2]([OH:4])=[O:3].[CH3:11][C:12]1[O:17][NH:16][C:14](=[O:15])[C:13]=1[CH2:18][CH:19]([NH2:23])[C:20]([OH:22])=[O:21]>>[CH2:1]([NH:5][CH2:6][P:7]([OH:10])([OH:9])=[O:8])[C:2]([OH:4])=[O:3].[CH3:13][C:14]([N:5]([CH2:6][P:7]([OH:10])([OH:9])=[O:8])[CH2:1][C:2]([OH:4])=[O:3])=[O:15].[CH3:11][C:12]1[O:17][NH:16][C:14](=[O:15])[C:13]=1[CH2:18][CH:19]([NH2:23])[C:20]([OH:22])=[O:21]

参加物

5

反応物 2

HCID 1221alpha-AMINO-3-HYDROXY-5-METHYL-4-ISOXAZOLEPROPIONIC ACIDHCID 3496Glyphosate

生成物 3

HCID 1221alpha-AMINO-3-HYDROXY-5-METHYL-4-ISOXAZOLEPROPIONIC ACIDHCID 3496GlyphosateHCID 23510850N-Acetyl-N-(phosphonomethyl)glycine

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-dfd52f1b4a04492c84128af2e0151717
出典データセット
uspto-grants-2011_08
特許番号
US08003398B2

関連ノート

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