Simultaneous determination of multi-component mycotoxin contaminants in foods and feeds by ultra-performance liquid chromatography tandem mass spectrometry

2007 
Abstract The present study developed an improved analytical method for the simultaneous quantification of 17 kinds of Aspergillus , Fusarium and Penicillium mycotoxin contaminants in foods and feeds by ultra-performance liquid chromatography combined with electrospray ionization triple quadrupole tandem mass spectrometry (UPLC–MS/MS) under the multiple reaction monitoring (MRM) mode, and especially focused on the optimization of extraction, clean-up, UPLC separation and MS/MS parameters of analytes. Homogenized samples were sequentially extracted by 84% (v/v) of acetonitrile aqueous solution with the selected internal standard (zearalanone) spiking, SPE clean-up with Mycosep 226 Aflazon+ Multifunctional cartridges, filtration, concentration and secondary filtration. Using double sample injection method, the analytes were separated by UPLC BEH C 18 column (100 mm × 2.1 mm I.D., 1.7 μm), and eluted with ammonium acetate/methanol and aqueous ammonia/methanol for the ESI + and ESI − analysis, respectively. The 10 positive ions and 7 negative ions of mycotoxins were separated by gradient elution with the retention time of 6.5 and 4 min, respectively. The LOQ of selected analytes ranged from 0.01 to 0.70 μg kg −1 , which was lower than the criteria of EU, USA and other countries on the determination of the minimum limiting level of various mycotoxins in foods including baby foods and feed stuffs. Meanwhile, high correlation coefficients ( r 2  > 0.99) of 17 mycotoxins were obtained within their respective linear ranges (0.05–20 μg kg −1 for 10 positive ions and 0.5–50 μg kg −1 for 7 negative ions) and reasonable recoveries (70.6–119.0%) of them were also demonstrated in different spiked levels. This quantitative method has many advantages including simple pretreatment, rapid determination and high sensitivity, which could be applied to the determination and quantification of multi-component mycotoxin contaminants in complex matrixes. Meanwhile, the method successfully fulfilled the minimum limiting level requests from various countries.
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