Simultaneous Determination of Aflatoxins and Ochratoxin A in Bee Pollen by Low-Temperature Fat Precipitation and Immunoaffinity Column Cleanup Coupled with LC-MS/MS

• Published in: Food analytical methods Vol. 7; no. 3; pp. 690 - 696
• Main Authors: Xue, XiaoFeng, Selvaraj, Jonathan Nimal, Zhao, Liuwei, Dong, Haimin, Liu, Fengmao, Liu, Yang, Li, Yi
• Format: Journal Article
• Language: English
• Published: Boston Springer US 01.03.2014
• Subjects: Analytical Chemistry; Chemistry; Chemistry and Materials Science; Chemistry/Food Science; Food Science; Microbiology; Aflatoxins; Immunoaffinity column; Bee pollen; Ochratoxin A; Low-temperature fat precipitation
• ISSN: 1936-9751; 1936-976X
• DOI: 10.1007/s12161-013-9723-4

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.