UHPLC Analysis of Patulin in Cloudy Apple Cider on Titan™ C18 following SPE using SupelMIP® SPE - Patulin

UHPLC Analysis of Patulin in Cloudy Apple Cider on Titan™ C18 following SPE using SupelMIP® SPE - Patulin

Conditions

sample preparation Dilute cloudy apply juice with 2% acetic acid 1:1, sonicate mixture for 60 minutes, centrifuge 5 minutes at RCF 4750, use resulting supernatant for SPE cleanup
sample preparation other: (1) Reconstitute sample in 500 µl of 0.1% acetic acid (2) Vortex reconstitute at high speed for 60 seconds.
sample preparation Solid Phase Extraction
sample/matrix Sample Pretreatment: Dilute cloudy apply juice with 2% acetic acid 1:1, sonicate mixture for 60 minutes, centrifuge 5 minutes at RCF 4750, use resulting supernatant for SPE cleanup. (Sample: Cloudy Apple Juice (Apple Cider))
extraction process Dilute cloudy apply juice with 2% acetic acid 1:1, sonicate mixture for 60 minutes, (centrifuge 5 minutes at RCF 4750, use resulting supernatant for SPE cleanup)
SPE tube/cartridge SupelMIP(R) SPE-Patulin 100mg/3mLTubes, Pk/50 (52776-U)
condition 2 mL acetonitrile, 1 mL water, 1 ml/minute
sample addition 4 mL diluted matrix, 1 mL/2 minute
washing 2 mL sodium bicarbonate, 2 mL water, 0.5 mL diethyl ether, 1 ml/min
drying - 10" vacuum for 10 minutes (post 2 mL water wash)
elution 2 mL Ethyl acetate, 1 ml/min
eluate post-treatment Evaporate eluate to dryness at 40 C with 10 psi nitrogen stream
column Titan C18, 10 cm x 2.1 mm I.D., 1.9 µm particles (577124-U)
column temp. 30 C
mobile phase [A] Acetonitrile; [B] Water
gradient 95% B hold for 6 min at 0.3 ml/min, to 20% B in 0.1 min at 0.4 ml/min, hold at 20% B for 1.4 min at 0.4 ml/min, to 95% B in 0.1 min at 0.3 ml/min, hold 95% B at 0.3 ml/min for 2.4 minutes.
sample 30 ng/mL patulin in 0.1% acetic acid
injection 15 µl
detector UV 276, 16

Description

Analysis Note A pectinase-free sample preparation method was developed to determine patulin concentrations in cloudy apple juice. Sonication and centrifugation were used to release incurred patulin from matrix material and to separate solids and pectin from samples prior to SPE cleanup using SupelMIP SPE - Patulin with molecularly imprinted polymer technology. Rapid UHPLC separation was achieved on Titan C18 columns with highest-grade UHPLC solvents for the mobile phase.
Categories Analytical Chromatography, Mycotoxins
Featured Industry Food and Beverages
Legal Information Titan is a trademark of Sigma-Aldrich Co. LLC, SupelMIP is a registered trademark of Sigma-Aldrich Co. LLC
suitability application for SPE, application for UHPLC

Materials

     
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