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LC/MS/MS Analysis of Phosphonic Amino Acid Herbicides and Their Metabolites, including Glyphosate, Referencing to China National Standard GB 23200.122-2026 (SI-50 4D)

National Standard of China GB 23200.122-2026*, "National food safety standard - Determination of four pesticides including glyphosate and their metabolites residues in foods of plant origin - Liquid chromatography-tandem mass spectrometry method", specifies the use of a quaternary ammonium-modified polyvinyl alcohol-based anion-exchange column or a column with equivalent performance. In this application, LC/MS/MS analyses of four phosphonic acid amino acid herbicides, including glyphosate and glufosinate, and six of their metabolites were performed using IC SI-50 4D.
Note: Although the GB method specifies the use of water for the preparation of N-methylglyphosate stock standard solution, the N-methylglyphosate reagent used in this application was insoluble in water and was therefore dissolved in 1 M NaOH aqueous solution. All other analytical conditions conformed to the GB method.

Preparation of standard solutions

  1. 1.Dissolve N-methylglyphosate in 1 M NaOH aqueous solution and dissolve all other reagents in water to prepare individual stock standard solutions at 1000 mg/L.
  2. 2.Mix the stock standard solutions and dilute with water to prepare a mixed intermediate standard solution at 50 mg/L.
  3. 3.Dilute the mixed intermediate standard solution prepared in step 2 with water to prepare a mixed standard solution at 1 mg/L.

*The version at the time of the application acquisition.

Sample: 10 µL

(Sample solution) 1 µg/mL each
Phosphonic acid
AMPA; Aminomethylphosphonic acid
Ethephon
MPPA; 3-Methylphosphinicopropionic acid
N-Acetyl AMPA
Glyphosate
Glufosinate ammonium
N-Methyl glyphosate
N-Acetyl glyphosate
N-Acetyl glufosinate

Chromatograms of PFAS
Column
Shodex IC SI-50 4D (4.0 mm I.D x 150 mm)
Eluent
(A) H2O, (B) 200 mM NH4HCO3 + 30 mM NH3 aq.
 
 Gradient; 10 % B (0 to 0.5 min) to 40 % B (1 min) to 80 % B (4 min) to 82.5 % B (5 min) to 95 % B (6 to 12 min) to 10 % B (12.1 to 15 min)
Flow rate
0.6 mL/min
Detector
ESI-MS (negative, MRM)
Column temp.
40 ℃

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