Comparison of Clean-Up Methods for Ochratoxin A on Wine, Beer, Roasted Coffee and Chili Commercialized in Italy
Abstract
:1. Introduction
2. Results and Discussion
2.1. Evaluation of Clean-Up on Wine
2.2. Evaluation of Clean-Up on Beer
Clean-up method | Validation levels (µg/L) | Recovery (%) (n =6 ) | RSD (%) (n = 6) | LOD (µg/L) (n = 6) | LOQ (µg/L) (n = 6) | RSDs (%) (n = 9) |
---|---|---|---|---|---|---|
IAC | 2 | 84.03 | 19.22 | 0.14 | 0.48 | 20.15 |
10 | 102.24 | 15.51 | 17.33 | |||
20 | 93.07 | 10.53 | 11.96 | |||
MIP | 2 | 80.46 | 27.01 | 0.14 | 0.48 | 36.15 |
10 | 54.15 | 6.13 | 12.42 | |||
20 | 70.31 | 9.67 | 10.41 | |||
Mycospin™ | 2 | 73.54 | 13.68 | 0.88 | 2.95 | 16.55 |
10 | 77.76 | 21.65 | 15.11 | |||
20 | 80.34 | 12.81 | 16.01 | |||
Mycosep™ | 2 | 96.75 | 24.48 | 0.12 | 0.40 | 20.63 |
10 | 81.58 | 2.46 | 6.82 | |||
20 | 102.68 | 3.69 | 6.55 | |||
HLB SPE | 2 | 59.34 | 13.89 | 2.02 | 6.73 | 19.66 |
10 | 83.49 | 18.56 | 19.38 | |||
20 | 56.29 | 1.11 | 15.66 |
Clean-up method | Validation levels (µg/L) | Recovery (%) (n = 6) | RSD (%) (n = 6) | LOD (µg/L) (n = 6) | LOQ (µg/L) (n = 6) | RSDs (%) (n = 9) |
---|---|---|---|---|---|---|
IAC | 2 | 84.84 | 25.41 | 0.08 | 0.26 | 21.44 |
10 | 105.89 | 15.29 | 19.15 | |||
20 | 99.2 | 9.09 | 14.33 | |||
MIP | 2 | 62.99 | 30.25 | 0.29 | 0.97 | 33.14 |
10 | 78.5 | 53.62 | 44.22 | |||
20 | 75.98 | 16.64 | 23.10 | |||
Mycospin™ | 2 | 15.63 | 12.87 | 0.14 | 0.9 | 9.22 |
10 | 53.15 | 9.22 | 10.03 | |||
20 | 68.1 | 8.61 | 9.98 | |||
Mycosep™ | 2 | 67.65 | 27.58 | 0.27 | 0.48 | 31.69 |
10 | 61.86 | 3.71 | 7.59 | |||
20 | 66.35 | 14.1 | 13.97 | |||
HLB SPE | 2 | 7.16 | 4.52 | 0.26 | 0.87 | 5.42 |
10 | 27.15 | 8.53 | 15.96 | |||
20 | 36.34 | 23.89 | 27.10 |
2.3. Evaluation of Clean-Up on Coffee
Clean-up method | Validation levels (µg/kg) | Recovery (%) (n = 6) | RSD (%) (n = 6) | LOD (µg/kg) (n = 6) | LOQ (µg/kg) (n = 6) | RSDs (%) (n = 9) |
---|---|---|---|---|---|---|
IAC | 5 | 75.15 | 12.35 | 0.48 | 1.63 | 11.10 |
10 | 83.68 | 2.16 | 6.23 | |||
20 | 79.98 | 11.14 | 12.41 | |||
MIP | 5 | 89.21 | 15.83 | 0.08 | 0.29 | 18.10 |
10 | 82.31 | 1.99 | 3.15 | |||
20 | 84.78 | 5.5 | 5.73 | |||
Mycospin™ | 5 | 33.61 | 33.81 | 3.03 | 10.12 | 30.62 |
10 | 35.63 | 16.92 | 15.93 | |||
20 | 38.91 | 25.93 | 16.22 | |||
Mycosep™ | 5 | 50.33 | 1.55 | 0.99 | 3.31 | 5.33 |
10 | 49.98 | 12.8 | 15.11 | |||
20 | 54.74 | 8.64 | 14.33 | |||
HLB SPE | 5 | 71.51 | 26.34 | 0.22 | 0.74 | 30.94 |
10 | 40.15 | 35.26 | 35.01 | |||
20 | 43.91 | 20.14 | 21.95 |
2.4. Evaluation of Clean-Up on Chili
Clean-up method | Validation levels (µg/kg) | Recovery (%) (n = 6) | RSD (%) (n = 6) | LOD (µg/kg) (n = 6) | LOQ (µg/kg) (n = 6) | RSDs (%) (n = 9) |
---|---|---|---|---|---|---|
IAC | 2 | 75.20 | 5.20 | 2.27 | 7.55 | 7.17 |
10 | 75.10 | 9.34 | 11.49 | |||
20 | 91.70 | 2.23 | 7.13 | |||
MIP | 2 | 83.81 | 31.58 | 1.77 | 5.93 | 34.52 |
10 | 74.85 | 0.47 | 5.63 | |||
20 | 81.00 | 1.95 | 6.18 | |||
Mycospin™ | 2 | 53.23 | 11.68 | 2.12 | 7.08 | 14.66 |
10 | 65.14 | 18.66 | 21.46 | |||
20 | 69.33 | 7.96 | 15.37 | |||
Mycosep™ | 2 | 91.35 | 8.12 | 0.30 | 1.00 | 9.17 |
10 | 102.60 | 1.37 | 6.33 | |||
20 | 96.60 | 2.85 | 4.82 | |||
HLB SPE | 2 | 49.41 | 28.94 | 1.25 | 4.18 | 25.69 |
10 | 57.88 | 35.80 | 33.15 | |||
20 | 56.29 | 1.11 | 14.23 |
2.5. OTA Analysis in Commercial Food Samples
Matrix | Calibration range (µg/kg) | r2 |
---|---|---|
Wine | 0.2–20 | 0.9986 |
Beer | 0.2–20 | 0.9910 |
Coffee | 1–20 | 0.9986 |
Chili | 1–20 | 0.9997 |
Matrix | Positive/Total (%) | Average contamination ± SD in positive samples (µg/kg) | Distribution of samples (µg/kg) | |||
---|---|---|---|---|---|---|
LOD–2.0 | 2.0–5.0 | 5.0–15.0 | >15.0 | |||
Wine | 2/30 (6.7%) | 2.34 ± 0.35 | - | 2 | - | - |
Beer | 5/30 (16.7%) | 0.35 ± 0.06 | 5 | - | - | - |
Coffee | 8/30 (26.7%) | 1.03 ± 0.17 | 7 | 1 | - | - |
Chili | 12/30 (40.0%) | 8.45 ± 1.73 | 4 | 5 | 2 | 1 |
3. Experimental Section
3.1. Chemicals and Reagents
3.2. Sample Preparation
3.3. Clean-Up Steps
3.4. HPLC and LC-MS/MS Conditions
3.5. Validation
4. Conclusions
Acknowledgments
Conflicts of Interest
References
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Prelle, A.; Spadaro, D.; Denca, A.; Garibaldi, A.; Gullino, M.L. Comparison of Clean-Up Methods for Ochratoxin A on Wine, Beer, Roasted Coffee and Chili Commercialized in Italy. Toxins 2013, 5, 1827-1844. https://doi.org/10.3390/toxins5101827
Prelle A, Spadaro D, Denca A, Garibaldi A, Gullino ML. Comparison of Clean-Up Methods for Ochratoxin A on Wine, Beer, Roasted Coffee and Chili Commercialized in Italy. Toxins. 2013; 5(10):1827-1844. https://doi.org/10.3390/toxins5101827
Chicago/Turabian StylePrelle, Ambra, Davide Spadaro, Aleksandra Denca, Angelo Garibaldi, and Maria Lodovica Gullino. 2013. "Comparison of Clean-Up Methods for Ochratoxin A on Wine, Beer, Roasted Coffee and Chili Commercialized in Italy" Toxins 5, no. 10: 1827-1844. https://doi.org/10.3390/toxins5101827
APA StylePrelle, A., Spadaro, D., Denca, A., Garibaldi, A., & Gullino, M. L. (2013). Comparison of Clean-Up Methods for Ochratoxin A on Wine, Beer, Roasted Coffee and Chili Commercialized in Italy. Toxins, 5(10), 1827-1844. https://doi.org/10.3390/toxins5101827