RAFA 2022

Tips and Tricks to Quantify Emerging Toxins and Process Contaminants: Analyze Alternarias, Ergots, and Other Major Mycotoxins Simultaneously in Various Food Matrices, and Furan and Alkyfurans Utilizing SPME Arrow to Increase Sensitivity.

Analysis of Furan and Alkylfurans in Food Commodities Using Headspace SPME Arrow and GC-MS

Large Volume Injection of Pesticides Using Low-Pressure Gas Chromatography

Concurrent Solvent Recondensation Large Sample Volume splitless injection (CSR-LVSI, or LVI) is a sample technique that overcomes the limitation of the maximum sample volume to 1–2 µL valid for classical splitless injection. Low-Pressure Gas Chromatography is a novel technique that had been successfully used for pesticide screening and quantification. The LPGC configuration with the restrictor/guard column lends itself to the requirements of the CSR-LVSI and has a potential to improve the sensitivity and lower detection limits. Large volume injection of acetonitrile and acetonitrile–toluene samples were evaluated in range of 1–25 µL for peak shapes, and the relationship between the peak area and injection volume was established. The large volume injections (>10 µL) resulted in peak splitting when the acetonitrile was used. The later eluting peaks were more affected; furthermore, the effect of increased volume on the area for injecting larger than 10 µL was negligible. The calibration parameters were compared for 1 µL and 5 µL injection. The limits of detection and other parameters were comparable between the two injection volumes. This presentation will describe both CSR-LVSI and LPGC and demonstrate the applicability of combining these techniques using a variety of solvents.

Simultaneous Determination of Alternaria Toxins, Ergot Alkaloid Epimers, and Other Major Mycotoxins in Various Food Matrices by LC-MS/MS

Various food commodities are vulnerable to different types of fungal pathogens and could be contaminated with differential classes of mycotoxins as a result. It is ideal to implement a generic method for simultaneous determination of multi-mycotoxins in different food matrices or agricultural products. In this study, a simplified sample preparation procedure and a reliable LC-MS/MS analytical method was developed for comprehensive measurement of 38 regulated and emerging mycotoxins including 5 Alternaria toxins, 6 major ergot alkaloids and their corresponding epimers. Four different food matrices (baby wheat cereal, peanut, tomato puree, and blended flour) were chosen for method validation to demonstrate the applicability of this analytical method to a wide range of food types. Sample extraction was performed using a formic acid-acidified 80:20 acetonitrile:water solution followed by extract dry-down and reconstitution in a 50:50 water:methanol solution for injection analysis on a biphenyl LC column. Chromatographic analysis was performed using LC-MS friendly acidic mobile phases and completed with a short 11-minute cycling time for proper separation of ergot alkaloid epimers. Accurate quantification was achieved using matrix-matched calibration standards at the range of 0.4 to 400 μg/kg. The recoveries of all mycotoxins (except citrinin) in fortified samples were from 70% to 120%, and the relative standard deviation (RSD) was less than 20%. For the vast majority of analytes, the limit of quantification was at 0.4 μg/kg, which was satisfactory to meet the regulatory levels.