Development and comparison of single-step solid phase extraction and QuEChERS clean-up for the analysis of 7 mycotoxins in fruits and vegetables during storage by UHPLC-MS/MS

摘要

A robust and sensitive UHPLC-MS/MS method was developed for the analysis of seven mycotoxins in fruits and vegetables. The variations of seven mycotoxins concentrations during storage were also determined for the first time. Solid phase extraction (SPE) and QuEChERS clean-up were compared, and extraction was finally performed with acetonitrile under acidic conditions followed by HLB SPE purification. Seven mycotoxins were separated on a C18 column by gradient elution, scanned by ESI+ and ESI- dynamic switching and detected with MRM mode. LOD and LOQ, matrix effect, accuracy and precision of the developed method were investigated. Results were linear in their concentration ranges for all mycotoxins with R-2 being greater than 0.999. LODs and LOQs were ranged from 0.05 to 3.0 mu g/kg and 0.2 to 10.0 mu g/kg, respectively. Average recoveries were between 81.1% and 116% with intraday-and interday-precision being in the ranges of 3.0-6.2% and 4.2-6.1%, respectively. The validated method provides sufficient selectivity, sensitivity and accuracy to screen for seven mycotoxins at trace levels, without using standard addition or matrix-matched calibration to compensate for matrix effects. The method was successfully applied for mycotoxins analysis in fruits and vegetables. None were detected in fresh samples, but AOH and AME were detected in strawberry, and TeA was detected in tomato fruits during long-term storage. Their concentrations were in the range of 3.6-165.3 mu g/kg from 3 days to 60 days and significantly increased along with storage time.