[Simultaneous determination of aflatoxins, zearalenone and ochratoxin A in cereal grains by immunoaffinity column and high performance liquid chromatography coupled with post-column photochemical derivatization].
A method was developed for the simultaneous determination of aflatoxins (AFs) (B1, B2, G1 and G2), zearalenone (ZEA) and ochratoxin A (OTA) in cereal grains by high performance liquid chromatography (HPLC) with fluorescence detection after immunoaffinity column clean-up and post-column derivatization. Cereal grain sample was extracted with methanol-water (80: 20, v/v). The extract was purified by immunoaffinity column and the toxins were separated by reversed-phase HPLC, and quantified with fluorescence detection after photochemical derivatization. The separation was performed on a Nova-Pak column (3.9 mm i. d. x 150 mm, 4 microm, Waters) with a linear gradient of methanol-acetonitrile-1% phosphoric acid mixture. The calibration curves for mycotoxins were made in the concentration range of 0.24 - 6.0 for AFs ( B1, B2, G1 and G2), 4.0 - 100.0 for ZEA and 0.5 - 40.0 microg/L for OTA. Recoveries of the different cereal grains (wheat, rice, rye) spiked with mycotoxins at levels ranged from 0.24 -1.0 microg/kg for AFs (B1, B2, G1 and G2), 4.0 -16.0 microg/kg for ZEA and 0.5 - 3.0 microg/kg for OTA were from 70.8% to 94.0% and relative standard deviations were between 2.79% and 9.38%. The limits of detection were 0.24 Rg/kg for AFs (B1, B2, G1 and G2), 0.5 microg/kg for OTA and 4.0 microg/kg for ZEA.
Li
Jun
J
Liaoning Entry and Exit Inspection and Quarantine Bureau, Dalian 116001, China. lj666623@sina.com
Yu
Yimang
Y
Tian
Miao
M
Wang
Hongwei
H
Wei
Feng
F
Li
Li
L
Wang
Xiong
X
D000348:Aflatoxins / Q000032:analysis*; D002846:Chromatography, Affinity / Q000379:methods; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D056148:Chromatography, Reverse-Phase; D002523:Edible Grain / Q000737:chemistry*; D009793:Ochratoxins / Q000032:analysis*; D055668:Photochemical Processes; D015025:Zearalenone / Q000032:analysis*
D000348:Aflatoxins; D009793:Ochratoxins; C025589:ochratoxin A; D015025:Zearalenone