Automatic Pretreatment of Dispersive Liquid Liquid Microextraction Based on Immunomagnetic Beads Coupled with UPLC-FLD for the Determination of Zearalenone in Corn Oils.

Sample pretreatment is a vital step in the detection of mycotoxins, and traditional pretreatment methods are time-consuming, labor-intensive and generate much organic waste liquid. In this work, an automatic, high-throughput and environmentally friendly pretreatment method is proposed. Immunomagnetic beads technology and dispersive liquid-liquid microextraction technology are combined, and the zearalenone in corn oils is directly purified and concentrated under the solubilization effects of surfactant. The proposed pretreatment method allows for the batch pretreatment of samples without pre-extraction using organic reagents, and almost no organic waste liquid is produced. Coupled with UPLC-FLD, an effective and accurate quantitative detection method for zearalenone is established. The recovery of spiked zearalenone in corn oils at different concentrations ranges from 85.7 to 89.0%, and the relative standard deviation is below 2.9%. The proposed pretreatment method overcomes the shortcomings of traditional pretreatment methods and has broad application prospects.

A Study of a New Certified Reference Material for Accurate Determination of the Main Fusarium Mycotoxins in Whole-Wheat Flour.

Matrix certified reference materials (CRMs) play a critical role in analytical method validation and the assurance of reliable measurement results. A certified reference material (GBW(E)100813) for whole-wheat flour was developed to ensure an accurate and reliable measurement of the main Fusarium mycotoxins (deoxynivalenol (DON), nivalenol (NIV), deoxynivalenol-3-glucoside (DON-3G), and zearalenone (ZEN)). CRM candidates were prepared using sun-drying, grinding, sieving, homogenising, packaging, and gamma irradiation. The final produced CRM was packaged at 50 g per unit and stored at 20 °C. Certification was performed using isotope dilution-liquid chromatography-tandem mass spectrometry. CRM characterization was performed in eight laboratories in accordance with the requirements of ISO Guide 35. The certified values and expanded uncertainties (at a confidence of 95%, k = 2) for DON, NIV, DON-3G, and ZEN were determined to be 0.98 ± 0.12 mg/kg, 1.37 ± 0.20 mg/kg, 242 ± 35 µg/g, and 382 ± 50 µg/g. The CRM was sufficiently homogeneous between and within bottles, and remained stable for up to 12 months at 20 °C and 9 days below 40 °C for transportation. Thus, CRM can be used for quality control and method validation to ensure the accurate and reliable quantification of the main Fusarium mycotoxins in whole-wheat flour.