Using Solid-Phase Microextraction Coupled with Reactive Carbon Fiber Ionization-Mass Spectrometry for the Detection of Aflatoxin B1 from Complex Samples

Abstract

Aflatoxin B1 (AFB1) is a common mycotoxin present in agricultural and food products. Therefore, rapid screening methods must be developed for AFB1 detection with high sensitivity and good selectivity. In this study, we developed an analytical method based on the combination of solid-phase microextraction (SPME) with carbon fiber ionization (CFI)-mass spectrometry (MS) to detect the presence of trace AFB1 from complex samples. A pencil lead (type 2B, length: ~2.5 cm) with a sharp end (diameter: ~150 μm) was used as the SPME fiber and the ionization emitter in CFI-MS analysis. Owing to the graphite structure of the pencil lead, AFB1 can be trapped on the pencil lead through π–π interactions. After adsorbing AFB1, the pencil lead was directly introduced in a pipette tip (length: ~0.7 cm; tip inner diameter: ~0.6 mm), placed close (~1 mm) to the inlet of the mass spectrometer, and applied with a high voltage (−4.5 kV) for in situ AFB1 elution and CFI-MS analysis. A direct electric contact on the SPME-CFI setup was not required. Followed by the introduction of an elution solvent (10 μL) (acetonitrile/ethanol/deionized water, 2:2:1 (v/v/v)) to the pipette tip, electrospray ionization was generated from the elution solvent containing AFB1 for CFI-MS analysis. A reactive SPME-CFI-MS strategy was employed to further identify AFB1 and improve elution capacity using our approach. Butylamine was added to the elution solvent, which was then introduced to the pipette tip inserted with the SPME fiber. Butylamine-derivatized AFB1 was readily generated and appeared in the resultant SPME-CFI mass spectrum. The lowest detectable concentration against AFB1 using our approach was ~1.25 nM. Our method can distinguish AFB1 from AFG1 in a mixture and can be used for the detection of trace AFB1 in complex peanut extract samples.