Simultaneous Detection of 11 Mycotoxins in Aquatic Products using Multifunctional Column Clean-up and Ultrahigh-performance Liquid Chromatography-tandem Mass Spectrometry
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Abstract:
A novel method to simultaneously detect 11 kinds of mycotoxins (aflatoxin B1 [AFB1], aflatoxin B2 [AFB2], aflatoxin G1 [AFG1], aflatoxin G2 [AFG2], aflatoxin M1 [AFM1], ochratoxin A [OTA], zearalenone [ZEN], deoxynivalenol [DON], 3-acetyldeoxynivalenol [3-AcDON], 15-AcDON, and fusarenon-X [Fus-X]) in aquatic products was developed, using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with multiple reaction monitoring (MRM). The samples were extracted with acetonitrile-water (84:16, V/V), purified using a multifunctional clean-up column (MycoSpin 400), and separated by a chromatographic column (Waters Acquity UPLCTM BEH C18; 100 × 2.1 mm i.d., 1.7 μm) using (0.01% formic acid-0.05% ammonia-H2O)/methanol as mobile phase. The quantitative and qualitative analyses were conducted in MRM mode with a mass spectrometer and an external standard. The results indicated that 11 mycotoxins showed good linear relationship within their respective linear response ranges, the correlation coefficients were > 0.9918, the limit of quantitation (LOQ) was 0.1 to 20.0 μg/kg, and the average recoveries (n = 3) were from 62.8% to 115.3%, with values of relative standard deviation (RSD) ranging between 2.6% and 19.0%. The developed method with the facile pretreatment, good purification effect, high sensitivity and reproducibility can be used for rapid detection of trace levels of multiple mycotoxins in aquatic products.
