LC/MS Analysis of Glyphosate in Oatmeal on ApHera™ NH2 after SPE using Supel™ Select HLB

LC/MS Analysis of Glyphosate in Oatmeal on ApHera™ NH2 after SPE using Supel™ Select HLB

Conditions

sample/matrix instant oatmeal, ground
SPE tube/cartridge Supel-Select HLB SPE, 30 mg/1 ml (54181-U)
condition 1 mL methanol, 1 mL 50:50 methanol:water
sample addition 0.5 mL extract
elution collect the second loaded aliquot of the extract
eluate post-treatment filter into low absorption vials
column apHera NH2, 15 cm x 4.6 mm I.D., 5 µm particles (56401AST)
column temp. 35 °C
mobile phase [A] water; [B] 20 mM ammonium carbonate, pH 9; [C] methanol:water (50:50)
gradient 100% A for 2 min, to 90% B, 10% C in 0.1 min, held until 10 min, to 100% A in 0.1 min, held for 5 min
flow rate 0.5 mL/min
pressure 3191 psi (220 bar)
injection 60 µL
detector MS/MS, ESI negative, 168/63, 168/79

Description

Analysis Note Direct analysis of glyphosate with LC-MS detection using the presented method is possible for oat, corn and rice products. Polymeric SPE was used for sample cleanup. Polymer-based apHera NH2 HPLC column provided stable and robust separation at basic pH.
Categories Analytical Chromatography, Pesticides & Herbicides
Featured Industry Food and Beverages
Legal Information apHera is a trademark of Sigma-Aldrich Co. LLC, Supel is a trademark of Sigma-Aldrich Co. LLC
Other Notes Sample pretreatment: 5 g of homogenized cereal was mixed wtih 10 mL water and let sit for at least 30 minutes. 10 mL 1% (v/v) formic acid in acetonitrile was added, shaken for 15 minutes on a laboratory shaker, and centrifuged.5 g of homogenized cereal was mixed wtih 10 mL water and let sit for at least 30 minutes. 10 mL 1% (v/v) formic acid in acetonitrile was added, shaken for 15 minutes on a laboratory shaker, and centrifuged.
suitability application for LC-MS

Materials

     
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