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G005645

LC/MS/MS of Pesticides in Oranges on Ascentis® Express C18 after Sample Prep using Supel Que Z-Sep/C18 QuEChERS sorbent

application for HPLC

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technique(s)

HPLC: suitable

test parameters

sample preparation: Dispersive (QuEChERS)
sample/matrix: 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)
extraction tube: Supel QuE Citrate (EN) Tube (55227-U)
extraction process: 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
clean-up tube: Supel-Q PSA/C18 (55284-U)
clean-up process: 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.)
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 acetonitrile
gradient: 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
flow rate: 0.3 mL/min
pressure: 2730 psi (188 bar)
column temp.: 30 °C
detector: MS/MS, ESI positive

suitability

application for HPLC

application(s)

food and beverages

Analysis Note

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

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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