A Dilute and Shoot Strategy for Determining Alternaria Toxins in Tomato-Based Samples and in Different Flours Using LC-IDMS Separation
Abstract
:1. Introduction
2. Results
2.1. Analysis of Quality Control Samples Using the Optimized Method
2.2. Method Performance Characteristics
3. Discussion
3.1. LC–MS/MS Analysis of Alternaria Toxins
3.2. Method Application
4. Materials and Methods
4.1. Standards, Reagents, Equipment, and Samples
4.2. Sample Preparation
4.3. LC–IDMS Determination
4.4. Quantification
5. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Compounds | Precursor Ion (m/z) | Product Ion (m/z) | Dwell Time (ms) | DP (V) | EP (V) | CE (V) | CXP (V) | IR% in Solvent | IR% in Samples | PTL for Ion Ratio% (± 30%) |
---|---|---|---|---|---|---|---|---|---|---|
AOH | 257.1 | 215.1 | 50 | −60 | −10 | −35 | −15 | 73 | 69–80 | 51–95 |
212.1 | 50 | −35 | −8 | |||||||
AOH-d3 | 260.1 | 218.1 | 50 | −60 | −10 | −35 | −15 | - | – | – |
AME | 271.1 | 256.1 | 50 | −60 | −10 | −27 | −16 | 23 | 17–24 | 16–30 |
228.1 | 50 | −36 | −18 | |||||||
AME-d3 | 274.1 | 259.1 | 50 | −60 | −10 | −36 | −16 | - | – | – |
TEA | 196.0 | 139.0 | 50 | −50 | −10 | −27 | −9 | 64 | 60–72 | 45–83 |
112.0 | 50 | −30 | −9 | |||||||
TEA-13C2 | 198.0 | 141.1 | 50 | −50 | −10 | −27 | −9 | - | – | – |
TEN | 413.2 | 141.1 | 50 | −70 | −10 | −25 | −7 | 72 | 67–78 | 50–94 |
271.1 | 50 | −22 | −16 | |||||||
TEN-d3 | 416.2 | 274.1 | 50 | −70 | −10 | −22 | −16 | - | – | – |
ALT | 291.1 | 214.1 | 50 | −75 | −10 | −29 | −15 | 66 | 50–74 | 46–86 |
186.1 | 50 | −35 | −10 | |||||||
ALT-d6 | 296.1 | 189.1 | 50 | −75 | −10 | −35 | −10 | - | - | - |
Sample Code | Matrix | Detected Concentration | Trueness% | Detected Concentration | Trueness % | Detected Concentration | Trueness % | Detected Concentration | Trueness % | Detected Concentration | Trueness % |
---|---|---|---|---|---|---|---|---|---|---|---|
AOH | AME | TEA | TEN | ALT | |||||||
P49 | Naturally contaminated tomato puree | 25.6 µg/kg (27.4 ± 3.45) | 93.4 | 14.8 µg/kg (16.4 ± 1.89) | 90.2 | 997 µg/kg (961 ± 58.6) | 104 | - | - | - | - |
N22 | Naturally contaminated tomato puree | 11.7 µg/kg (12.9 ± 2.01) | 90.7 | 5.26 µg/kg (6.19 ± 0.68) | 85.0 | 460 µg/kg (499 ± 39.8) | 92.2 | - | - | - | - |
R61 | Naturally contaminated tomato puree | 5.88 µg/kg (6.06 ± 0.86) | 97.0 | 2.34 µg/kg (2.69 ± 0.32) | 87.0 | 182 µg/kg (183 ± 11.5) | 99.4 | - | - | - | - |
Y21 | Spiked tomato puree | 1.39 µg/kg (1.82 ± 0.26) | 76.4 | 1.45 µg/kg (1.98 ± 0.26) | 73.2 | 45.1 µg/kg (47.0 ± 4.88) | 96.0 | 50.1 µg/kg (44.9 ± 4.21) | 111 | 1.69 µg/kg (2.18 ± 0.41) | 77.5 |
H60 | Spiked tomato puree | 9.16 µg/kg (9.68 ± 1.33) | 94.6 | 8.56 µg/kg (9.74 ± 0.86) | 87.9 | 201 µg/kg (194 ± 16.1) | 104 | 225 µg/kg (218 ± 34.4) | 103 | 10.1 µg/kg (11.2 ± 1.86) | 90.2 |
B56 | Naturally contaminated wheat | 1.54 µg/kg (2.04, not evaluated in the trial) | 75.5 | 0.63 µg/kg (0.55, not evaluated in the trial) | 115 | 282 µg/kg (265 ± 19.7) | 106 | 55.7 µg/kg (52.2 ± 6.68) | 107 | - | - |
G28 | Naturally contaminated wheat | 1.52 µg/kg (1.83 ± 0.50) | 83.1 | 0.68 µg/kg (1.29 ± 0.34) | 52.7 | 145 µg/kg (162 ± 14.4) | 89.5 | 3.44 µg/kg (5.29 ± 1.31) | 65.0 | - | - |
Compound | AOH | AME | TEA | TEN | ALT |
---|---|---|---|---|---|
Tomato | |||||
Absolute recovery% (n = 10) | 66.7–75.4 | 67.6–74.6 | 75.7–91.6 | 87.3–88.7 | 82.9–89.0 |
Precision (RSD%) | 2.8–6.3 | 1.0–3.5 | 1.7–2.5 | 2.6–5.5 | 4.1–7.6 |
Absolute ME% (ESTD) | 23.8–48.7 ion suppression | 0.4–6.8 ion suppression | 0.6–4.9 ion suppression | 0.8–7.2 ion suppression | 6.6–7.7 ion enhancement |
Relative ME% (ESTD) | 20.8 | 4.8 | 4.5 | 6.4 | 0.32 |
Absolute ME% (ISTD) | 4.9–9.7 ion suppression | 0.5–7.3 ion suppression | 2.0–6.5 ion suppression | 1.3–3.7 ion suppression | 2.6–7.5 ion suppression |
Relative ME% (ISTD) | 3.2 | 5.2 | 4.1 | 2.7 | 0.56 |
LOQ (µg/kg) | 0.20 | 0.02 | 0.50 | 0.10 | 0.50 |
Flour | |||||
Absolute recovery% (n = 10) | 69.0–76.3 | 68.1–75.1 | 77.7–90.0 | 87.8–89.2 | 84.5–89.0 |
Precision (RSD%) | 3.2–7.7 | 1.9–4.9 | 0.8–2.8 | 3.5–4.6 | 7.7–8.3 |
Absolute ME% (ESTD) | 62.0–53.9 ion suppression | 18.4–25.6 ion suppression | 0.1–10.3 ion suppression | 21.6–35.8 ion suppression | 48.3–66.3 ion suppression |
Relative ME% (ESTD) | 10.1 | 5.0 | 5.1 | 10.4 | 6.8 |
Absolute ME% (ISTD) | 2.3–6.8 ion suppression | 1.0–4.1 ion suppression | 0.7–1.4 ion suppression | 0.2–5.9 ion suppression | 5.4–9.9 ion suppression |
Relative ME% (ISTD) | 5.2 | 2.6 | 0.4 | 3.0 | 2.6 |
LOQ (µg/kg) | 0.20 | 0.04 | 0.70 | 0.15 | 0.80 |
Sample Availability: Samples of the compounds are not available from the authors. |
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Tölgyesi, Á.; Farkas, T.; Bálint, M.; McDonald, T.J.; Sharma, V.K. A Dilute and Shoot Strategy for Determining Alternaria Toxins in Tomato-Based Samples and in Different Flours Using LC-IDMS Separation. Molecules 2021, 26, 1017. https://doi.org/10.3390/molecules26041017
Tölgyesi Á, Farkas T, Bálint M, McDonald TJ, Sharma VK. A Dilute and Shoot Strategy for Determining Alternaria Toxins in Tomato-Based Samples and in Different Flours Using LC-IDMS Separation. Molecules. 2021; 26(4):1017. https://doi.org/10.3390/molecules26041017
Chicago/Turabian StyleTölgyesi, Ádám, Tamás Farkas, Mária Bálint, Thomas J. McDonald, and Virender K. Sharma. 2021. "A Dilute and Shoot Strategy for Determining Alternaria Toxins in Tomato-Based Samples and in Different Flours Using LC-IDMS Separation" Molecules 26, no. 4: 1017. https://doi.org/10.3390/molecules26041017