Analysis of wheat extracts for ochratoxin A by molecularly imprinted solid-phase extraction and pulsed elution

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Abstract
A molecularly imprinted solid-phase extraction (MISPE) method has been developed for the rapid analysis of wheat extracts for ochratoxin A (OTA). Molecularly imprinted polymer (MIP) particles were synthesized from N-phenylacrylamide (PAM) and slurry-packed into a micro-column for selective solid-phase extraction (SPE) of OTA. With water flowing at 0.5 mL min−1, a total binding capacity of 30 ng OTA was determined for the 20 mg of MIP particles. MISPE conditions were optimized using OTA in methanol/acetic acid (99:1 v/v). Nearly 100% binding could be achieved from one 20-μL injection of sample containing up to 30 ng of OTA. Pulsed elution (PE) using methanol/triethylamine (99:1 v/v) was good for the quantitative desorption of OTA. The MISPE–PE method, with fluorescence detection at λ ex=385 nm and λ em=445 nm, afforded a detection limit of 5.0 ng mL−1 (or 0.1 ng in 20 μL of sample injected) for OTA. Recovery of OTA from wheat extracts was 103±3%. Each MISPE–PE analysis required less than 5 min to complete.

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