Fe₃O₄@PDA/MIL‐101(Cr) as magnetic solid‐phase extraction sorbent for mycotoxins in licorice prior to ultrahigh‐performance liquid chromatography‐tandem mass spectrometry analysis

Abstract

Magnetic solid‐phase extraction (MSPE) strategy based on the Fe3O4@PDA/MIL‐101(Cr) has been proposed to separate and purify five common mycotoxins in licorice, including aflatoxin B1, aflatoxin G1, sterigmatocystin, zearalenone, and ochratoxin A. Integrating the MSPE and solid–liquid extraction/partitioning, a modified QuEChERS was established to adapt to the complex licorice samples. The Fe3O4@PDA/MIL‐101(Cr) was successfully synthesized and characterized by Fourier transform infrared spectroscopy (FT‐IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and nitrogen adsorption–desorption isotherms. Sorbents with superior advantages for exclusion of matrix interference and extraction of target analytes in a short time were obtained, according to their ability of magnetic separation, high surface area (287.75 m2/g), large pore volume (0.61 cm3/g), and nanosized structure with mesopores. Prior to analysis with ultrahigh‐performance liquid chromatography‐tandem mass spectrometry (UHPLC‐MS/MS), several key parameters that would affect the sorbents’ extraction efficiency were extensively investigated. Under the optimized conditions, the practicality of the developed method for analysis of mycotoxins in licorice samples was confirmed by adequate linearity (R2 ≥ 0.9967), high sensitivity (LODs and LOQs, respectively, in the ranges 0.01–0.09 and 0.02–0.30 μg/kg), acceptable recovery (78.53%–116.28%), satisfactory reusability, and good interbatch precision of the sorbents (RSDs in the ranges 6.70%–11.20% and 6.02%–10.35%, respectively). The results indicated that the established method was feasible and reliable for the environment‐friendly and rapid screening of mycotoxins in complex licorice samples.

Use of polypyrrole ferrite microparticles and liquid chromatography-mass spectrometry for testing natural grass contamination by multiclass mycotoxins

“…As shown in Table S4, the Fe 3 O 4 @PPy microcomposite had one of the best performances in the determination of multiclass mycotoxins, allowing the preconcentration of 13 mycotoxins and being one of the two methods that allowed the simultaneous determination of more mycotoxins and the only one that allowed the determination of DON, T-2, and HT-2 toxins, in addition to the main aflatoxins and the emerging mycotoxins. Furthermore, sample preparation time (25 min) is comparable or better than extraction times previously reported, which are in the 15 min to 1 h and 10 min range [26][27][28][29][30]. In terms of analysis results, it can be observed that the proposed method showed comparable or higher validation parameters to the previously reported methods for other magnetic adsorbents.…”

“…So far, different nanomaterials have been used for the determination of specific groups of mycotoxins, including multiwalled carbon nanotubes for AFB 1 and ZEN extraction from wheat flour and for main aflatoxins (AFs) (aflatoxins B 1 , B 2 , G 1 and G 2 ). In addition, other multi-walled carbon nanotubes based materials have also been used for the determination of aflatoxins M 1 (AFM 1 ) and M 1 (AFM 2 ), OTA, ZEN, zearalanone (ZAN), α-zeralanol, β-zeralanol, α-zeralenol and β-zeralenol in liquid milk [26,27], as well as coreshell nanomaterials in the form of covalent or metal-organic frameworks for the analysis of maize (AFs, ochratoxins and ENNs) or liquorice (AFG 1 , AFB 1 , sterigmatocystin, ZEN and OTA) [28,29]. Other magnetic nanoparticles (MNPs) based on ferrite cores with nonporous silica shell have been used for fumonisin B1, ZEN, and OTA preconcentration from vegetable oil [30], or with cellulose shell for ENNs and BEA from paprika samples [31].…”

Solid‐phase extraction techniques based on nanomaterials for mycotoxin analysis: An overview for food and agricultural products

“…So far, m‐SPE represents one of the most exploited SPE techniques in numerous fields [111]. Comparatively speaking, literature about the application of m‐SPE in mycotoxin analysis is much more than that of D‐μ‐SPE, involving magnetized carbon nanoparticles [112–119], functionalized magnetic nanoparticles [120–140], and magnetized nanoporous materials [141–149].…”

“…The sorbent's highly stable and selective enrichment performance was assumed to result from the high specificity of the aptamers and the maximized aptamer coverage density provided by MIL‐101@Fe 3 O 4 . Our group fabricated MIL‐101(Cr)‐PDA@Fe 3 O 4 and applied it to isolate and purify AFB 1 , AFG 1 , STER, ZEN, and OTA from licorice [149]. MIL‐101(Cr) was synthesized directly around the PDA‐functionalized Fe 3 O 4 .…”

Fe3O4@COF(TAPT–DHTA) Nanocomposites as Magnetic Solid-Phase Extraction Adsorbents for Simultaneous Determination of 9 Mycotoxins in Fruits by UHPLC–MS/MS

“…The following supporting information can be downloaded at: . References [ 16 , 38 , 39 , 40 , 41 , 42 , 43 ] are cited in the supplementary materials. Table S1.…”