LC/MS/MS Analysis of Carbendazim in Orange Juice (Spiked) on Ascentis® Express C18 after Supel™ QuE PSA/C18 QuEChERS Cleanup
Materials
analytical column
SPE tube or plate
CONDITIONS
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
Description
Analysis Note
Simple and fast extraction and analytical method were developed for analysis of fungicide carbendazim in orange juice samples. QuEChERS extraction method was used with PSA/C18 cleanup. Ascentis Express C18 column chromatography was coupled to MS/MS detection with limits of detection at 0,1 ppb.
Legal Information
Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany
Supel is a trademark of Sigma-Aldrich Co. LLC
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