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Simultaneous Determination of Aflatoxins and Ochratoxin A in Bee Pollen by Low-Temperature Fat Precipitation and Immunoaffinity Column Cleanup Coupled with LC-MS/MS |
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| Authors: | XiaoFeng Xue Jonathan Nimal Selvaraj Liuwei Zhao Haimin Dong Fengmao Liu Yang Liu Yi Li |
| Affiliation: | 1. Bee Research Institute, Chinese Academy of Agricultural Sciences, Beijing, 100093, People’s Republic of China 3. Risk Assessment Laboratory for Bee Products Quality and Safety of Ministry of Agriculture,, Beijing, 100093, People’s Republic of China 2. Department of Food Safety and Quality Control, Key Laboratory of Agro-products processing comprehensive laboratory, Ministry of Agriculture, Institute of Agro-products Processing Science and Technology, Chinese Academy of Agricultural Sciences, Beijing, 100193, People’s Republic of China 4. Department of Applied Chemistry, College of Science, China Agricultural University, Beijing, 100193, China |
| Abstract: | A simple and sensitive method has been developed for simultaneous determination of aflatoxins (AFB1, AFB2, AFG1, and AFG2) and ochratoxin A (OTA) in bee pollen. The analytes in the sample were extracted with a mixture of acetonitrile/water (60:40, v/v), using low temperature for fat precipitation, followed by immunoaffinity column cleanup of extracts. The mycotoxins were quantified using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) with an electrospray ionization (ESI) and a triple quadrupole (QqQ) analyzer. Matrix effect, accuracy, and precision were evaluated and achieved good results calculated by matrix-matched calibration standards which reduced the influence of matrix effect. Recoveries at three levels were in the range of 74.3–96.5 % with RSD less than 10.0 %. The correlation coefficients (r 2) of the five mycotoxins were higher than 0.997. The method showed high sensitivity with LOD below 0.05 μg/kg. |
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