Highly selective and sensitive high performance liquid chromatography method for determination of fumonisins from feed samples with MIL-101 based dispersed micro-solid-phase extraction and precolumn fluorescence derivatization

A selective and rapid high-performance liquid chromatography with fluorescence detection (HPLC-FLD) method for determining fumonisins was established and validated, which based on dispersed microsolid-phase extraction (D-mu -SPE) and precolumn derivatization. The MIL-101 was prepared as sorbents to selectively enrich two fumonisins from feed samples. The obtained extracts were labeled by a novel derivatization reagent 2,5-dioxo-pyrrolidin-1-yl 4-(1-methyl-1H-phenanthro[9,10-d]imidazol-2-yl)benzoate (MPIBA-Su). There was no fluores-cence from fumonisins itself, while their derivatives exhibited considerable fluorescence with a maximum excitation at lambda ex 255 nm and a maximum emission at lambda em 457 nm. Key factors affecting extraction efficiency and derivatization efficiency were fully optimized. Excellent linearity was achieved with correlation coefficients > 0.9935 under optimal conditions. The detection limits (LODs) were between 2.4 and 3.5 ng center dot mL(-1), and the quantitation limits (LOQs) were between 8.1 and 11.7 ng center dot mL(-1). With recoveries in the range of 83.8% -94.3%, the established method has successfully been applied to the quantitative analysis of fumonisins in feed samples.

Automated summary

A selective and rapid HPLC-FLD method based on D-mu -SPE and precolumn derivatization was established for determining fumonisins. The method utilized MIL-101 as sorbents to selectively enrich fumonisins from feed samples, and the labeled extracts showed strong fluorescence. The method achieved excellent linearity and sensitivity, and was successfully applied to the analysis of fumonisins in feed samples.