LC/MS/MS Analysis of Neonicotinoid Pesticides in Dandelion Blossoms on Ascentis® Express C18 after Dispersive SPE (QuEChERS) using Supel™ QuE

LC/MS/MS Analysis of Neonicotinoid Pesticides in Dandelion Blossoms on Ascentis® Express C18 after Dispersive SPE (QuEChERS) using Supel™ QuE

Conditions

sample preparation Dispersive (QuEChERS)
sample/matrix 3 g pulverized dandelion blossoms, homogenized in 10 mL water
extraction tube Supel QuE Acetate extration tube (55234-U)
extraction process add 25 mL of acetonitrile; add contents of Supel QuE acetate extraction tube; shake immediately for 1 minute; centrifuge at 3400 rpm for 5 minutes
clean-up process Transfer 1 mL of the acetonitrile layer into a Supel QuE PSA/C18 cleanup tube; shake for 1 minute; centrifuge at 3500 rpm for 3 minutes; (draw off 700 uL of supernatant, evaporate to dryness at 50 C under nitrogen; reconstitute in 200 µl of 50:50 0.1% formic acid:0.1% formic acid in methanol)
clean-up tube Supel QuE PSA/C18 tube (55288-U)
column Ascentis Express C18, 10 cm x 3.0 mm I.D., 2.7 µm particles (53814-U)
column temp. 25 C
mobile phase [A] 0.1% formic acid in water; [B] 0.1% formic acid in methanol
gradient 30% B from 0 to 5 min; to 100% B in 0.2 min; held at 100% B for 5.3 min; to 30% B in 0.5 min; held at 30% B for 5 min
flow rate 500 µL/min
pressure 3800 psi (262 bar)
injection 3 µl
detector MS, ESI(+), MRM, m/z 203.2/129.2, 271.2/225.0, 292.1/211.0, 256.0/175.2, 250.0/132.0, 223.2/126.0, 253.0/125.8

Description

Analysis Note The advent of the die-off of honey bees due to colony collapse disorder (CCD) has spawned investigation into pesticide exposure as the cause. Neonicotinoids are among the suspected culprits. In this application, the QuEChERS approach using Supel QuE was used for extraction and cleanup prior to analysis of seven neonicotinoid pesticides in flower blossoms. Ascentis® Express C18 was chosen due to the high efficiency associated with its Fused-Core® particle, and its relatively low backpressure as compared to sub-2 micron UHPLC columns. This allowed the column to be used in a standard pressure HPLC system with a relatively high concentration of aqueous at the start of the mobile phase gradient.
Categories Analytical Chromatography, SPE Applications, Pesticides & Herbicides, Pesticides
Featured Industry Agriculture
Legal Information Ascentis is a registered trademark of Sigma-Aldrich Co. LLC, Supel is a trademark of Sigma-Aldrich Co. LLC, Fused-Core is a registered trademark of Advanced Materials Technology, Inc.
suitability application for HPLC

Materials

     
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