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LC/MS/MS Analysis of Aflatoxins in Hops on Ascentis® Express 2.7 μm Phenyl-Hexyl after Cleanup Using Supel™ Tox AflaZea SPE

LC/MS/MS Analysis of Aflatoxins in Hops on Ascentis® Express 2.7 μm Phenyl-Hexyl after Cleanup Using Supel™ Tox AflaZea SPE

Conditions

sample preparation dilute 0.2 mL of the extract with 0.8 mL distilled water and mix well
sample/matrix hops extract was spiked with aflatoxins at corresponding concentrations of 6 ppb each (for Aflatoxin B2 and G2) and 24 ppb each (for Afltoxin B1 and G1) in hops
extraction process 0.5 g of finely ground hops is mixed with 10 mL of 84:16 acetonitrile:water for 30 minutes, centrifuged
SPE tube/cartridge Supel Tox AflaZea SPE, 6 mL (55314-U)
sample addition 2 mL of hops sample extract
elution apply strong vacuum and collect the sample into plastic tube
column Ascentis Express Phenyl-Hexyl, 5 cm x 2.1 mm I.D., 2.7 µm particles (53334-U)
column temp. 40 C
mobile phase [A] 5 mM ammonium formate with 1% formic acid in water; [B] 5 mM ammonium formate with 1% formic acid in methanol
gradient 30% B to 60% B in 3 min; to 100% B in 2 in; held at 100% B for 2 min; to 30% B in 0.1 min; held at 30% B for 1.4 min
flow rate 0.4 ml/min
pressure 5511 psi (380 bar)
injection 10 µl
detector MS, ESI(+), MRM 331.3/189.0, 329.1/243.0, 315.9/259.0, 313.1/241.0

Description

Analysis Note The complex composition of hops makes it difficult to apply sample cleanup methods commonly used for other commodities. In this application, interference removal on Supel Tox AflaZea SPE was used for sample cleanup providing quick and effective sample preparation prior to separation on an Ascentis Express Phenyl-Hexyl column and mass spectrometric detection. It is recommended to use silanized glass vials for this analysis.
Categories Analytical Chromatography, Herbal medicines
Featured Industry Food and Beverages
Legal Information Ascentis is a registered trademark of Sigma-Aldrich Co. LLC, Supel is a trademark of Sigma-Aldrich Co. LLC
Other Notes Use silanized vials for analysis.
suitability application for LC-MS, application for SPE

Materials

     
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