Investigation of Twelve Significant Mycotoxin Contamination in Nut-Based Products by the LC–MS/MS Method
Abstract
:1. Introduction
2. Results
3. Discussion
4. Materials and Methods
4.1. Samples Collection
4.2. Sample Preparation
4.3. LC–MS/MS Procedure
4.4. Total Aerobic Mesophilic Bacteria (TAMB) Analysis
4.5. Statistical Analyses
5. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Mycotoxins | Chocolate Brands | ||
---|---|---|---|
A | B | ||
AFB1 | N (Positive/Total) | 10/10 | nd |
Mean ± S.E (μg/kg) | 0.18 ± 0.02 | nd | |
Min (μg/kg) | 0.11 | nd | |
Max (μg/kg) | 0.24 | nd | |
AFG1 | N (Positive/Total) | 10/10 | nd |
Mean ± S.E (μg/kg) | 0.23 ± 0.01 | nd | |
Min (μg/kg) | 0.17 | nd | |
Max (μg/kg) | 0.27 | nd | |
OTA | N (Positive/Total) | 10/10 | 10/10 |
Mean ± S.E (μg/kg) | 1.87 a ± 0.11 | 0.44 b ± 0.07 | |
Min (μg/kg) | 1.20 | 0.13 | |
Max (μg/kg) | 2.34 | 0.68 | |
STE | N (Positive/Total) | 8/10 | nd |
Mean ± S.E (μg/kg) | 1.01 ± 0.14 | nd | |
Min (μg/kg) | 0.49 | nd | |
Max (μg/kg) | 1.50 | nd | |
ZON | N (Positive/Total) | 10/10 | nd |
Mean ± S.E (μg/kg) | 3.11 ± 0.64 | nd | |
Min (μg/kg) | 0.90 | nd | |
Max (μg/kg) | 7.57 | nd | |
DON | N (Positive/Total) | 1/10 | 10/10 |
Mean ± S.E (μg/kg) | 29.52 | 29.81 ± 2.77 | |
Min (μg/kg) | 29.52 | 11.81 | |
Max (μg/kg) | 29.52 | 42.09 |
Mycotoxins | Hazelnut Butters | ||
---|---|---|---|
C | D | ||
AFB1 | N (Positive/Total) | 4/10 | 6/10 |
Mean ± S.E (μg/kg) | 1.03 ± 0.72 | 0.21 ± 0.07 | |
Min (μg/kg) | 0.27 | 0.04 | |
Max (μg/kg) | 3.18 | 0.49 | |
AFB2 | N (Positive/Total) | 4/10 | 2/10 |
Mean ± S.E (μg/kg) | 0.12 ± 0.03 | 0.08 ± 0.01 | |
Min (μg/kg) | 0.06 | 0.07 | |
Max (μg/kg) | 0.20 | 0.08 | |
AFG1 | N (Positive/Total) | 2/10 | 5/10 |
Mean ± S.E (μg/kg) | 0.17 ± 0.005 | 0.22 ± 0.05 | |
Min (μg/kg) | 0.16 | 0.14 | |
Max (μg/kg) | 0.17 | 0.40 | |
OTA | N (Positive/Total) | 2/10 | 3/10 |
Mean ± S.E (μg/kg) | 0.59 ± 0.35 | 0.05 ± 0.02 | |
Min (μg/kg) | 0.24 | 0.01 | |
Max (μg/kg) | 0.94 | 0.08 | |
STE | N (Positive/Total) | 1/10 | 2/10 |
Mean ± S.E (μg/kg) | 0.23 | 0.66 ± 0.44 | |
Min (μg/kg) | 0.23 | 0.22 | |
Max (μg/kg) | 0.23 | 1.09 | |
T2 | N (Positive/Total) | 3/10 | 3/10 |
Mean ± S.E (μg/kg) | 1.75 ± 0.19 | 2.09 ± 0.23 | |
Min (μg/kg) | 1.41 | 1.77 | |
Max (μg/kg) | 2.08 | 2.54 | |
ZON | N (Positive/Total) | 2/10 | 3/10 |
Mean ± S.E (μg/kg) | 2.41 ± 1.14 | 0.98 ± 0.48 | |
Min (μg/kg) | 1.27 | 0.33 | |
Max (μg/kg) | 3.55 | 1.91 | |
HT2 | N (Positive/Total) | 2/10 | 2/10 |
Mean ± S.E (μg/kg) | 7.01 b ± 0.07 | 7.42 a ± 0.02 | |
Min (μg/kg) | 6.94 | 7.40 | |
Max (μg/kg) | 7.07 | 7.43 |
Mycotoxins | Peanut Butter Brands | ||||
---|---|---|---|---|---|
E | F | G | H | ||
AFB1 | N (Positive/Total) | 10/10 | 10/10 | 10/10 | 10/10 |
Mean ± S.E (μg/kg) | 5.37 ± 2.20 | 13.35 a ± 2.37 | 8.11 b ± 1.56 | 0.94 c ± 0.24 | |
Min (μg/kg) | 0.18 | 5.56 | 1.02 | 0.20 | |
Max (μg/kg) | 22.97 | 27.37 | 15.67 | 2.89 | |
AFB2 | N (Positive/Total) | 10/10 | 10/10 | 10/10 | 10/10 |
Mean ± S.E (μg/kg) | 0.93 ± 0.36 | 2.53 a ± 0.60 | 1.54 b ± 0.28 | 0.20 c ± 0.03 | |
Min (μg/kg) | 0.08 | 0.87 | 0.28 | 0.10 | |
Max (μg/kg) | 3.86 | 6.19 | 3.02 | 0.46 | |
AFG1 | N (Positive/Total) | nd | 2/10 | nd | nd |
Mean ± S.E (μg/kg) | nd | 0.21 ± 0.03 | nd | nd | |
Min (μg/kg) | nd | 0.18 | nd | nd | |
Max (μg/kg) | nd | 0.24 | nd | nd | |
FB2 | N (Positive/Total) | nd | nd | 5/10 | nd |
Mean ± S.E (μg/kg) | nd | nd | 2.85 ± 0.04 | nd | |
Min (μg/kg) | nd | nd | 2.73 | nd | |
Max (μg/kg) | nd | nd | 2.93 | nd | |
OTA | N (Positive/Total) | 10/10 | 10/10 | 10/10 | 8/10 |
Mean ± S.E (μg/kg) | 2.87 ± 1.85 | 7.02 ± 3.39 | 4.43 ± 0.92 | 0.17 ± 0.05 | |
Min (μg/kg) | 0.19 | 1.72 | 0.51 | 0.09 | |
Max (μg/kg) | 19.20 | 37.26 | 9.26 | 0.47 | |
STE | N (Positive/Total) | 5/10 | 10/10 | 3/10 | 0/10 |
Mean ± S.E (μg/kg) | 0.40 b ± 0.11 | 1.23 a ± 0.19 | 0.57 ± 0.17 | nd | |
Min (μg/kg) | 0.19 | 0.47 | 0.26 | nd | |
Max (μg/kg) | 0.83 | 2.25 | 0.86 | nd | |
ZON | N (Positive/Total) | nd | 2/10 | 1/10 | nd |
Mean ± S.E (μg/kg) | nd | 0.08 ± 0.05 | 0.24 | nd | |
Min (μg/kg) | nd | 0.03 | 0.24 | nd | |
Max (μg/kg) | nd | 0.12 | 0.24 | nd |
TAMB | Positive Samples (%) | Number of Positive Samples | Mean ± S.E (log CFU/g) |
---|---|---|---|
Chocolates | 50 | 10 | 2.41 ± 0.08 |
Hazelnut butters | 5 | 1 | 2.73 |
Peanut butters | 80 | 32 | 2.74 ± 0.06 |
Total | 53.75 | 43 | 2.66 ± 0.05 |
TAMB | Peanut Butters | |||
E | F | G | H | |
N (Positive/Total) | 3/10 | 10/10 | 10/10 | 9/10 |
Mean ± S.E (log CFU/g) | 2.23 c ± 0.04 | 2.90 a ± 0.09 | 2.89 b ± 0.10 | 2.57 ± 0.10 |
Min (log CFU/g) | 2.15 | 2.54 | 2.48 | 2.15 |
Max (log CFU/g) | 2.30 | 3.43 | 3.59 | 3.12 |
TAMB | Chocolates | Nut Butters | ||
A | B | C | D | |
N (Positive/Total) | 7/10 | 3/10 | 0/10 | 1/10 |
Mean ± S.E (log CFU/g) | 2.52 a ± 0.07 | 2.15 b ± 0.00 | <102 | 2.73 |
Min (log CFU/g) | 2.24 | 2.15 | <102 | 2.73 |
Max (log CFU/g) | 2.77 | 2.15 | <102 | 2.73 |
Mycotoxins | Nut Butter | Chocolate | ||||||||
---|---|---|---|---|---|---|---|---|---|---|
RSD (%) | Rec (%) | LOD (µg/kg) | LOQ (µg/kg) | R2 | RSD (%) | Rec (%) | LOD (µg/kg) | LOQ (µg/kg) | R2 | |
AFB1 | 3.84 | 96.15 | 0.03 | 0.09 | 0.997 | 2.95 | 98.38 | 0.02 | 0.18 | 0.998 |
AFB2 | 3.23 | 94.62 | 0.02 | 0.08 | 0.997 | 3.94 | 88.92 | 0.03 | 0.32 | 0.998 |
AFG1 | 2.44 | 95.15 | 0.02 | 0.06 | 0.998 | 4.87 | 101.88 | 0.02 | 0.18 | 0.993 |
AFG2 | 11.24 | 101.55 | 0.09 | 0.29 | 0.993 | 3.51 | 101.55 | 0.01 | 0.11 | 0.995 |
DON | 4.62 | 110.68 | 3.83 | 12.77 | 0.999 | 4.24 | 102.69 | 2.38 | 23.77 | 0.992 |
FB1 | 3.81 | 74.13 | 2.12 | 7.07 | 0.999 | 5.22 | 53.18 | 0.65 | 6.51 | 0.998 |
FB2 | 2.33 | 83.89 | 1.47 | 4.89 | 0.998 | 1.79 | 76.75 | 0.19 | 1.88 | 0.998 |
HT2 | 3.19 | 111.40 | 2.66 | 8.88 | 0.999 | 12.63 | 86.54 | 1.43 | 14.31 | 0.997 |
OTA | 6.32 | 95.20 | 0.01 | 0.15 | 0.995 | 4.3 | 98.91 | 0.02 | 0.19 | 0.997 |
STE | 2.29 | 94.16 | 0.02 | 0.05 | 0.994 | 3.53 | 100.04 | 0.01 | 0.15 | 0.998 |
T2 | 2.96 | 95.55 | 0.21 | 0.71 | 0.994 | 2.98 | 95.52 | 0.14 | 1.38 | 0.998 |
ZON | 4.40 | 94.78 | 0.03 | 0.11 | 0.996 | 1.78 | 102.33 | 0.11 | 1.12 | 0.999 |
Mycotoxins | RT | Parent Ion (m/z) | Fragment Ions | Concentration Range (µg/L) | Ion Mode | Fragmentor Voltage (V) | CE (V) | |
---|---|---|---|---|---|---|---|---|
AFB1 | 4.89 ± 0.01 | 313 | 285/240.9 | 0.05–1 | Positive | 130 | 22 | 38 |
AFB2 | 4.76 ± 0.01 | 315 | 287/258.9 | 0.05–1 | Positive | 140 | 24 | 30 |
AFG1 | 4.70 ± 0.03 | 329 | 242.9/200 | 0.05–1 | Positive | 120 | 26 | 38 |
AFG2 | 4.55 ± 0.02 | 331 | 312.9/245 | 0.05–1 | Positive | 120 | 24 | 30 |
DON | 4.09 ± 0.05 | 297 | 249/231 | 5–100 | Positive | 80 | 4 | 6 |
FB1 | 4.13 ± 0.05 | 722.1 | 352.1/334.1 | 5–100 | Positive | 180 | 36 | 40 |
FB2 | 4.61 ± 0.01 | 706.2 | 336.1/318 | 1.5–30 | Positive | 190 | 40 | 42 |
HT2 | 5.95 ± 0.01 | 442.1 | 263/215 | 5–100 | Positive | 90 | 3 | 3 |
OTA | 5.47 ± 0.01 | 404 | 358/239 | 0.05–1 | Positive | 100 | 10 | 20 |
STE | 5.97 ± 0.02 | 325 | 309.9/280.9 | 0.05–1 | Positive | 130 | 24 | 38 |
T2 | 5.46 ± 0.01 | 484.2 | 215/185 | 0.5–10 | Positive | 90 | 14 | 16 |
ZON | 5.72 ± 0.01 | 317 | 174.9/130.9 | 0.5–10 | Negative | 130 | 12 | 20 |
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Er Demirhan, B.; Demirhan, B. Investigation of Twelve Significant Mycotoxin Contamination in Nut-Based Products by the LC–MS/MS Method. Metabolites 2022, 12, 120. https://doi.org/10.3390/metabo12020120
Er Demirhan B, Demirhan B. Investigation of Twelve Significant Mycotoxin Contamination in Nut-Based Products by the LC–MS/MS Method. Metabolites. 2022; 12(2):120. https://doi.org/10.3390/metabo12020120
Chicago/Turabian StyleEr Demirhan, Buket, and Burak Demirhan. 2022. "Investigation of Twelve Significant Mycotoxin Contamination in Nut-Based Products by the LC–MS/MS Method" Metabolites 12, no. 2: 120. https://doi.org/10.3390/metabo12020120
APA StyleEr Demirhan, B., & Demirhan, B. (2022). Investigation of Twelve Significant Mycotoxin Contamination in Nut-Based Products by the LC–MS/MS Method. Metabolites, 12(2), 120. https://doi.org/10.3390/metabo12020120