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Fipronil is a pesticide that is used in many countries around the world. It is effective against a large number of agricultural pests, but also has a harmful effect on humans above certain levels. It is suspected of being carcinogenic. The use of fipronil in food-producing animals is prohibited.
Chemically speaking, fipronil belongs to the phenylpyrazole group. It is practically insoluble in water, but shows good solubility in polar organic solvents such as acetone or ethyl acetate. Fipronil is an optically active substance, i.e. fipronil is present in two mutually enantiomeric forms. These can be separated using chiral HPLC. However, fipronil is used as a racemate (as a mixture of enantiomers in a 1:1 ratio).
Fipronil is often analysed using liquid or gas chromatography coupled to a mass spectrometer (LC-MS or GC-MS). The QuEChERS method is often used for sample preparation.
Column: Astec (R,R) P-CAP 250x4.6mm, 5µm (31024AST)
Mobile phase: 80/20 heptane/ethanol
Flow rate: 1 mL/min
Temperature: 25 °C
Detection: UV, 235 nm
Sample: 1 mg/mL in methanol
1. fipronil
Column: Kromasil Eternity 2.5-C18 50x4.6mm (EH2CLA05)
Mobile phase: 70/30/0.2 acetonitrile/water/acetic acid
Flow rate: 1 mL/min
Temperature: 40 °C
Detection: UV, 260 nm
1. triflurlin 2. impurity 3. propyzamide 4. primicarb 5. chlorpiriphos-methyl 6. pyrimiphos-ethyl 7. fipronil 8. Dazomet isomer 9. Dazomet isomer 10. fluazifop-p-butyl 11. fenazaquin 12. benfuracarb 13. impurity 14. azoxystrobin
Column: SLB-5ms 10m x 0.1mm, 0.1 µm (28465-U)
Temperature: 40 °C (1 min), 80 °C/min to 160 °C, 5 °C/min to 340 °C (2 min)
Injection temperature: 280 °C
MSD interface: 280 °C
Carrier gas: Helium, 0.52 mL/min
Injection: 0.5 µL, 10:1 split
Sample: each analyte 0.8-2 µg/mL in 50/50 hexane/acetone
HPLC - Chiral separation:
Gas chromatography:
HPLC - Reversed Phase:
HPLC - Reversed Phase:
Sample preparation:
HPLC - Reversed Phase:
HPLC - Chiral separation:
Gas chromatography:
HPLC - Reversed Phase:
UHPLC - Reversed Phase
Gas chromatography:
Sample preparation:
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