Zhongguo shipin weisheng zazhi (Jan 2020)
Determination of aflatoxins and zearalenone in vegetable oil and cereal products by solid phase extraction column purification coupled with ultra-performance liquid chromatography tandem mass spectrometry
Abstract
Objective To develop a method for simultaneous determination of aflatoxins (AFs) and zearalenone (ZEN) in vegetable oil and cereal products by solid phase extraction column purification coupled with ultra-performance liquid chromatography tandem mass spectrometry (UPLC). Methods AFs and ZEN in vegetable oil were extracted by acetonitrile-water solution (90:10, V:V). AFs and ZEN in cereals were firstly extracted by acetonitrile-acetic acid-water solution (84:1:16, V:V) and then extracted by dichloromethane/ethyl acetate (90:10, V:V), and the extracts were concentrated and reconstructed by acetonitrile-water solution (90:10, V:V). The extracts of vegetable oil/cereals were purified by C18-Al2O3 solid phase extraction column. AFs and ZEN were separated by UPLC with acetonitrile-water gradient elution in a CORTECSTM C18 chromatography column (2.1 mm×100 mm, 2.7 μm), and qualified/quantified by mass spectrometry with electron spray ionization multiple reaction monitoring mode with stable-isotope internal standard. Results The linearity of AFs and ZEN were 0.1-30.0 and 1.0-500.0 ng/ml, the limits of detection were 0.03 and 0.3 μg/kg, and the limits of quantification were 0.10 and 1.0 μg/kg, respectively. The average recoveries of AFs and ZEN for spiked samples was 68.3%-98.6% and 84.5%-108.0% with the relative standard deviation 4.6%-11.5% and 4.2%-9.0% (n=6), respectively. Several quality control material were analyzed to verified the accuracy of the method.100 samples sold in Dalian markets were analyzed. Aflatoxin B1 and ZEN was detected in peanut oil and corn oil samples with maximum contents 12.80 and 370.00 μg/kg, respectively. Conclusion The method had several advantages including accurate, simple and cost-effective, environment friendly and it was applicable to batch analysis of AF and ZEN in vegetable oil and cereal products.
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