Conference Abstract Book

Analytical method development – QuEChERS*-LC-MS/MS DON AFB1 AFB2 AFG1 AFG2 OTA ZEA 0 20 40 60 80 100 Recovery (%) 0 200 400 600 800 1000 0 300 600 900 1200 1500 0 10 20 30 40 0 100 200 300 400 500 600 0 50 100 150 200 250 300 0 300 600 900 1200 1500 0 5 10 15 20 0 100 200 300 400 0 5 10 15 20 0 50 100 150 200 250 300 350 0 5 10 15 20 0 50 100 150 200 250 300 0 5 10 15 20 0 50 100 150 200 Analyte area DON (ng/ml) Plot Solvent Matrix Intercept -6.73787± 14.8823 Slope 1.37122± 0.03255 0.99413± 0.02243 Residual Sum of Squares 3851.15877 1245.55376 Pearson's r 0.99859 0.99898 R-Square (COD) 0.99719 0.99797 Adj. R-Square 0.99663 0.99746 y = 0.99x + 39.20, R² = 0.998 y = 1.37x ‒ 6.74, R² = 0.997 Analyte area OTA (ng/ml) Plot Solvent Matrix Intercept -0.19224± 2.37624 -0.39697± 2.42484 Slope 13.13156± 0.12995 13.274± 0.13261 Residual Sum of Squares 98.1821 102.23903 Pearson's r 0.99976 0.99975 R-Square (COD) 0.99951 0.9995 Adj. R-Square 0.99941 0.9994 y = 13.13x ‒ 0.19, R² = 0.999 y = 13.27x ‒ 0.39, R² = 0.999 Solvent-mached calibration curve Matrix-matched calibration curve Analyte area ZEA (ng/ml) Solvent Matrix -5.59435± 8.34324 -4.05912± 3.14365 4.39818± 0.06084 3.58724± 0.02292 1210.37758 171.83847 0.99952 0.9999 0.99904 0.9998 0.99885 0.99976 y = 4.40x ‒ 5.59, R² = 0.999 y = 3.59x ‒ 4.06, R² = 0.999 Analyte area AF B1 (ng/ml) Solvent Matrix -1.72082± 4.09709 -1.57576± 2.05295 15.52964± 0.44811 6.35084± 0.20791 291.87886 42.7945 0.99792 0.99786 0.99585 0.99573 0.99502 0.99466 y = 15.53x ‒ 1.72, R² = 0.996 y = 6.35x ‒1.58, R² = 0.996 Analyte area AF B2 (ng/ml) Equation y= a+ b*x Plot Solvent Matrix Intercept 7.15776± 4.94202 -8.81818± 1.8707 Slope 16.03294± 0.54053 9.90168± 0.18945 Residual Sum of Squares 424.67878 35.53356 Pearson's r 0.99717 0.99927 R-Square (COD) 0.99435 0.99854 Adj. R-Square 0.99322 0.99817 y = 16.03x + 7.16, R² = 0.994 y = 9.90x ‒ 8.82, R² = 0.999 Analyte area AF G1 (ng/ml) Plot Solvent Matrix Intercept 6.037± 3.62055 4± 1.53777 Slope 13.17711± 0.39599 7.17778± 0.15574 Residual Sum of Squares 227.92922 24.01111 Pearson's r 0.99775 0.99906 R-Square (COD) 0.9955 0.99812 Adj. R-Square 0.99461 0.99765 y = 13.18x + 6.04, R² = 0.996 y = 7.18x + 4.00, R² = 0.998 Analyte area AF G2 (ng/ml) Plot Solvent Matrix Intercept -0.56504± 6.20549 5.44309± 3.74115 Slope 10.05285± 0.57419 5.98374± 0.34617 Residual Sum of Squares 194.65041 70.74797 Pearson's r 0.99514 0.99502 R-Square (COD) 0.99031 0.99006 Adj. R-Square 0.98708 0.98675 y = 5.98x + 5.44, R² = 0.998 y = 10.05x ‒ 0.57, R² = 0.991 LC−MS/MS selected ion monitoring (SIM) chromatogram of the analytes Average recoveries of mycotoxins within the studied ranges solvent-matched & matrix-matched calibration curves μg/Kg AF B1 10 Sum AF B1,B2, G1 & G2 40 ΟΤΑ 20 DON 500 ZEA 150 Selected levels of dough contamination 1 2 3 *QuEChERS: "Qu ick, E asy, Ch eap, E ffective, R ugged, and S afe “ 2 g of extraction salts (FAL-QuEChERS® CMS4), consisting of 1.25 g MgSO 4 , 0.30 g NaCl, 0.30 g TCD, and 0.15 g DHSQ. Requirements 1. Consistent recoveries 2. Extract concentration within the range of the matrix-based calibration curves 66-100%