31P NMR

sample dissolved in Tris-EDTA (pH 8.0)

reference capillary 10 mM glufosinate ammonium in D2O (δP = 42.4 ppm)

(prepared by dissolving 19.8 mg in 10.0 mL D2O)

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Premier BEH Amide column

sample dissolved in MeCN:water (1:1)

A: H2O with 10 mM ammonium carbonate (NH4)2CO3 (961 mg in 1 L) and 0.04% ammonium hydroxide (2.0 mL of 20% solution), pH 9.7-9.8

B: MeCN

10% A for 2 min, 10-60% A over 10 min, 60% A for 2 min, 60-10% A over 0.5 min, 10% A for 5.5 min, posttime equilibration 10% A for 10 min

0.5 mL/min

negative ion mode 60-2000 amu

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Hypercarb column

sample dissolved in water

A: H2O with 0.5% FA

B: MeCN with 0.5% FA

2-20% B over 10 min, 20-100% B over 0.1 min, 100% B for 1.9 min, 100-2% B over 0.1 min, 2% B for 2.9 min

1.0 mL/min

positive ion mode 50-2000 amu

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