Dispersive (QuEChERS)
10 g of pureed oranges (homogenized with rind); spike at 50 ppb (add 16.75 μL of a custom made pesticide mix, each analyte at 30 μg/mL)
Supel™ QuE Citrate (EN) Tube (55227-U)
add 10 mL acetonitrile; shake for 1 minute; add contents of a Supel QuE citrate extraction tube (55227-U); shake immediately for 1 minute; centrifuge at 3200 rpm for 5 minutes
Supel-Q™ PSA/C18 (55284-U)
transfer 0.7 mL of the acetonitrile layer into a Supel QuE Z-Sep/C18 cleanup tube (55284-U); shake for 1 minute; centrifuge at 5000 rpm for 5 minutes; (transfer 0.2 mL of the supernatant into an empty 1.5 mL centrifuge tube; add 0.2 mL of water; centrifuge at 5000 rpm for 2 minutes.)
Ascentis Express C18, 5 cm x 2.1 mm I.D., 2.7 μm particles (53822-U)
[A] 10 mM ammonium acetate in water; [B] 10 mM ammonium acetate in acetonitrile
Hold at 30% B for 1 min; 30% to 80% B in 2 min; hold at 80% B for 4 min; hold at 100% B for 3 min; hold at 30% B for 3 min
0.3 mL/min
2730 psi (188 bar)
30 °C
MS/MS, ESI positive
This demonstrates the application of the Z-Sep/C18 sorbent to the cleanup of fruits in the LC-MS-MS analysis of polar pesticides including organophosphates, carbamates and benzoylureas
Sample pretreatment: 10 g of pureed oranges homogenized with rind; spike at 50 ppb by adding 16.75 μL of a pesticide mix containing each analyte at 30 μg/mL
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