3,4-Dimethylpyrazole phosphate (DMPP) is a nitration inhibitor added to solid fertilizers. The Japanese regulation for “Testing Methods for Fertilizers (2022*)” mentions to use an octadecylsilylated silica gel column for DMPP analysis. A calibration curve for DMPP obtained using Silica C18M 4D showed a high linearity with a coefficient of determination (R2) 0.9999 in the concentration range 0.5 to 50 μg/mL.
Urea fertilizer, one of the target fertilizers, was analyzed. The extract was prepared in accordance with the Testing Methods for Fertilizers. DMPP was not detected in the extract of the fertilizer analyzed. As a next step, addition recovery test was performed using the same sample (spiked DMPP concentration 0.185 mg/g). A good result was obtained with an average recovery rate of 102 % (n=3).
*The version at the time of the application acquisition.
- (1)Measure 1.00 g of urea fertilizer and put it in a 200-mL erlenmeyer flask. (For the spike recovery test DMPP was added to the sample at this point.)
- (2)Add 100 mL of water to (1) and stir with a magnetic stirrer for 10 minutes.
- (3)After allowing it to stand, transfer a portion of the supernatant to a 1.5-mL glass-stoppered centrifugal sedimentation tube.
- (4)Centrifuge (8000 ~ 10000 x g for about 5 minutes) and use the supernatant as an injection sample.
Sample: 10 µL
Standard solution (5 µg/mL)
Sample solution spiked with DMPP (0.185 mg/g)
Sample solution
- 1.DMPP (3,4-dimethylpyrazole phosphate)
- Column
- :Shodex Silica C18M 4D (4.6 mm I.D x 150 mm)
- Eluent
- :10 mM NaH2PO4 aq./CH3CN=1000/175
- Flow rate
- :0.7 mL/min
- Detector
- :UV (224 nm)
- Column temp.
- :40 ℃
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Applications
- Mild Hydrolysates of Allosamidin (ES-502C 7C)
- 5-(Hydroxymethyl)Furfural in Fruit Juice (ODP-50 6D)
- Cyanate and Carbamyl Phosphate (ES-502N 7C)
- Hydrogen Peroxide (KS-801)
- Chelating Reagents (1) (I-524A)
- Chelating Reagents (2) (NI-424)
- Analysis of Chelating Agents (ODP-50 4D)
- Hydantoins (DE-613)
- Amides (2) (Comparison of Reversed Phase Columns)
- Amides (3) (DE-413)
- Amides (4) (DE-413)
- Amides (5) (DE-413)
- Aldehydes (DE-413)
- Analysis of Humic Substances by SEC (SB-805 HQ)
- DNPH Derivative Aldehydes (ODP-50 4D)
- Analysis of Pochonicine and Its Analogues in Filamentous Fungi Culture Extract (ES-502C 7C)
- Separation of Furfural and Guaiacol (DE-413)
- Separation of C1 Compounds (DE-413)
- Simultaneous Analysis of Various Nitrogen Compounds According to Japanese Testing Methods for Fertilizers (ES-502C 7C)
- Separation of Substances Produced During Utilization of Biomass (VN-50 4D)
- LC/MS Analysis of Hexamethylenetetramine (VC-50 2D)