Comparative assessment of three extraction procedures for determination of emerging Fusarium mycotoxins in pasta by LC-MS/MS

A new rapid, sensitive, reproducible and reliable method was developed for the quantitative determination of enniatins A, A1, B and B1, beauvericin and fusaproliferin in dry and fresh pasta by liquid chromatography-triple quadrupole-tandem mass spectrometry. A comparative study of different rapid and economical extraction procedures was performed for the extraction of these mycotoxins in pasta. For this purpose, three different approaches were studied during the extraction step (Ultra-Turrax, ultrasonic bath and microwave). Optimal extraction conditions were reached using Ultra-Turrax with acetonitrile for 3 min without purification step. The chromatographic separation of the six mycotoxins was accomplished in 15 min. The method was extensively validated with satisfactory results: recovery rates ranged from 86 to 112% and the relative standard deviations were lower than 15%. Limits of detection ranged from 0.02 to 0.15 μg kg−1. The applicability of the method was assessed with the analysis of 30 samples of dry and fresh pasta.

► Validation a new LC-MS/MS method for the analysis of ENs, BEA and FUS. ► Sub-ppb LODs were obtained for all compounds. ► Comparison of three techniques for the extraction of ENs, BEA and FUS. ► Determination of ENs, BEA and FUS in commercial samples of pasta.