LC/MS/MS Analysis of Carbendazim in Orange Juice (Spiked) on Ascentis^® Express C18 after Supel^™ QuE PSA/C18 QuEChERS Cleanup

sample preparation

Dispersive (QuEChERS)

sample/matrix

orange juice spiked with carbendazim at 1 ppb

extraction tube

Supel^™ QuE Citrate (EN) Tube (55227-U)

extraction process

add 10 mL of orange juice with pulp to a 50 mL empty extraction tube (55248-U); add carbendazim at 1 ppb; add 10 mL acetonitrile; (shake for 1 minute; add contents of citrate extraction tube (55227-U); shake for 1 min; centrifuge at 3200 rpm for 5 minutes)

clean-up tube

Supel-Q^™ PSA/C18 (55288-U)

clean-up process

transfer 0.7 mL of the acetonitrile layer to the PSA/C18 cleanup tube (55288-U); shake 1 minute; (centrifuge for 3 minutes at 3400 rpm; remove 0.25 mL of the supernatant; mix with 0.25 mL water for LC-MS analysis)

column

Ascentis Express C18, 5 cm x 2.1 mm I.D., 2.7 μm particles (53822-U)

mobile phase

[A] 10 mM ammonium acetate in water; [B] 10 mM ammonium acetate in methanol

gradient

0-1 min: 30% B; 1.5-3.5 min: 100% B; 3.5-7 min: 30% B

flow rate

0-1 min: 0.3 mL/min; 1.5-7 min: 0.5 mL/min

column temp.

30 °C

detector

MS, ESI(+), MRM, m/z 192/160, 192/132

injection

5 μL