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How different microfilters affect the recovery of eleven EU-regulated mycotoxins

Marija Kovač Tomas
Marija Kovač Tomas
, 
Anto Mijatović
Anto Mijatović
, 
Mateja Bulaić Nevistić
Mateja Bulaić Nevistić
, 
Bojan Šarkanj
Bojan Šarkanj
, 
Jurislav Babić
Jurislav Babić
 et 
Tihomir Kovač
Tihomir Kovač
   | 04 avr. 2023
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Article Category: Original article
Publié en ligne: 04 avr. 2023
Pages: 8 - 15
Reçu: 01 nov. 2022
Accepté: 01 mars 2023
DOI: https://doi.org/10.2478/aiht-2023-74-3693
© 2023 Marija Kovač Tomas et al., published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Figure 1

Chemical structures of EU-regulated mycotoxins (excluding ergot alkaloids)
Chemical structures of EU-regulated mycotoxins (excluding ergot alkaloids)

Figure 2

Microfiltrate preparation. Filtrate solutions (vials) 1 and 2 were injected into the UHPLC column one at a time
Microfiltrate preparation. Filtrate solutions (vials) 1 and 2 were injected into the UHPLC column one at a time

Figure 3

UHPLC-MS/MS chromatogram of the selected EU-regulated mycotoxins in the unfiltered multi-mycotoxin standard solution (AFB1/AFG1 0.5 ng/mL, AFB2/AFG2 0.125 ng/mL, DON 50 ng/mL, FB1/FB2 37.5 ng/mL, ZEA 7.5 ng/mL, T-2/HT-2 2.5 ng/mL and OTA 0.25 ng/mL) obtained with an Acquity H-class – Xevo TQ-S micro system
UHPLC-MS/MS chromatogram of the selected EU-regulated mycotoxins in the unfiltered multi-mycotoxin standard solution (AFB1/AFG1 0.5 ng/mL, AFB2/AFG2 0.125 ng/mL, DON 50 ng/mL, FB1/FB2 37.5 ng/mL, ZEA 7.5 ng/mL, T-2/HT-2 2.5 ng/mL and OTA 0.25 ng/mL) obtained with an Acquity H-class – Xevo TQ-S micro system

Figure 4

Recoveries of mycotoxins with various filter membrane materials in filtrate solution 1 and 2 relative to the recovery (dashed line) from the unfiltered multi-mycotoxin solution. Low recoveries indicating mycotoxin loss during filtration are framed in squares. CA – cellulose acetate; MCE – mixed cellulose ester; NY – nylon; PES – polyethersulphone; PTFE – polytetrafluoroethylene
Recoveries of mycotoxins with various filter membrane materials in filtrate solution 1 and 2 relative to the recovery (dashed line) from the unfiltered multi-mycotoxin solution. Low recoveries indicating mycotoxin loss during filtration are framed in squares. CA – cellulose acetate; MCE – mixed cellulose ester; NY – nylon; PES – polyethersulphone; PTFE – polytetrafluoroethylene

Figure 5

Relative recovery of the 11 mycotoxins in filtrate solutions 1 and 2 by filter membrane material. CA – cellulose acetate; FS1 – filtrate solution 1 (first three drops of the solution); FS2 – filtrate solution 2 (the rest of the solution); MCE – mixed cellulose ester; NY – nylon; PES – polyethersulphone; PTFE – polytetrafluoroethylene
Relative recovery of the 11 mycotoxins in filtrate solutions 1 and 2 by filter membrane material. CA – cellulose acetate; FS1 – filtrate solution 1 (first three drops of the solution); FS2 – filtrate solution 2 (the rest of the solution); MCE – mixed cellulose ester; NY – nylon; PES – polyethersulphone; PTFE – polytetrafluoroethylene

Figure 6

Relative recovery of the “outlier” mycotoxins AFB2 (a) and HT-2 (b) from filtrate solutions 1 and 2 by filter membrane materials. CA – cellulose acetate; FS1 – filtrate solution 1 (first three drops of the solution); FS2 – filtrate solution 2 (the rest of the solution); MCE – mixed cellulose ester; NY – nylon; PES – polyethersulphone; PTFE – polytetrafluoroethylene
Relative recovery of the “outlier” mycotoxins AFB2 (a) and HT-2 (b) from filtrate solutions 1 and 2 by filter membrane materials. CA – cellulose acetate; FS1 – filtrate solution 1 (first three drops of the solution); FS2 – filtrate solution 2 (the rest of the solution); MCE – mixed cellulose ester; NY – nylon; PES – polyethersulphone; PTFE – polytetrafluoroethylene

MS/MS parameters for mycotoxin analysis

Mycotoxin Precursor ionm/z Cone voltageV Collision energyV Product ionsm/z
AFB1 313.2 (M+H)+ 60 38 241.0
23 285.3
AFB2 315.2 (M+H)+ 60 30 259.0
25 287.0
AFG1 329.2 (M+H)+ 60 28 311.0
24 243.0
AFG2 331.2 (M+H)+ 60 24 313.0
28 245.1
DON 297.2 (M+H)+ 25 10 249.0
10 203.2
FB1 722.4 (M+H)+ 50 40 334.3
40 352.3
FB2 706.4 (M+H)+ 50 40 336.2
40 318.2
ZEA 317.1 (M–H)- -58 30 131.0
20 175.0
T-2 484.7 (M+NH4)+ 25 20 185.0
25 215.0
HT-2 442.6 (M+NH4)+ 25 10 263.4
15 215.3
OTA 404.1 (M+H)+ 30 24 239.0
14 358.0

Preparation of the multi-mycotoxin standard solution

Analyte Concentration of analytical standard (μ/mL) Volume of analytical standard for preparation of 1000 μL of combined multi-mycotoxin standard solution* (μL) Concentration of combined multi-mycotoxin standard solution (ng/mL) Concentration of 100× diluted combined multi-mycotoxin standard solution (ng/mL)
DON 100 50 5000 50
AFB1 2.0 25 50 0.5
AFB2 0.5 25 12.5 0.125
AFG1 2.0 25 50 0.5
AFG2 0.5 25 12.5 0.125
FB1 50 75 3750 37.5
FB2 50 75 3750 37.5
ZEA 100 7.5 750 7.5
T-2 100 2.5 250 2.5
HT-2 100 2.5 250 2.5
OTA 10 2.5 25 0.25
Volume of combined multi-mycotoxin standard solution for preparation of 1000 μL of 100× diluted combined multi-mycotoxin standard solution** (μL) 10
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