1 An HPLC-MS/MS Method Using a Multitoxin Clean-up Column for Analysis of Seven Mycotoxins in Aquafeeds.

Background In Guangdong Province of China, the climate here is very wet, so there are many different fungus living in the aquatic feeds, which produce mycotoxins. These compounds contaminate agriculture products world-wide and represent a great threat to human health. It is necessary to determine their contamination level in aquatic feeds. Objective A high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method was developed for the quantitative analysis of aflatoxin B1, aflatoxin M1, T-2 toxin, HT-2 toxin, deoxynivalenol, ochratoxin, and zearalenone in the fish and shrimp feed. Methods Samples were extracted with acetonitrile-water (V: V = 3:1), and degreased with acetonitrile-saturated hexane. Such obtained extract was cleaned up with a multitoxin column. The target compounds were separated on a C18 chromatographic column and analyzed simultaneously by electrospray ionization mass spectrometry in both positive or negative ion mode. Detected compounds were quantified by using the matrix-matched external standard method. Results Under the optimized conditions, good linearities for the analytes in corresponding concentration range were obtained with correlation coefficients (r2) higher than 0.9948. LOD ranged from 1.83 to 12.63 μg/kg, and LOQ ranged from 5.49 to 37.89 μg/kg. Average recoveries for the target mycotoxins at three spiked levels ranged from 80.5% to 116.5% with RSD ranging from 2.4% to 10.4%. 23 real aquafeed samples were determined by this method, and 7 kinds of toxins were all detected. Conclusions Obtained results showed that developed method could be successfully applied for the simultaneous determination of mycotoxins in aquatic feeds.