Survey on Antibiotic Residues in Egg Samples in Italy
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals, Reagents, Stock, and Intermediate Solutions
2.2. Chromatographic Conditions
2.3. MS Conditions
2.4. Sample Preparation
2.5. Method Validation
2.6. Real Samples Analysis
2.7. Risk Exposure
3. Results and Discussion
3.1. Sample Preparation
3.2. Method Validation
3.3. Real Samples Analysis
3.4. Risk Exposure
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Analyte | Class | Mean Recovery (%) | CVr (%) | CVwR (%) | CCα (µg kg−1) | LOD (µg kg−1) | LOQ (µg kg−1) | ME a (%) |
---|---|---|---|---|---|---|---|---|
Florfenicol amine | Amphenicols | 74 | 9.0 | 9.8 | 3.3 | 3.3 | 3.3 | 3 |
Thiamphenicol b | 77 | 8.9 | 11 | 10 | 3.3 | 10 | −9 | |
Florfenicol b | 80 | 8.1 | 11 | 10 | 3.3 | 10 | −17 | |
Desacetyl cephapirin | Cephalosporins | 74 | 8.6 | 9.7 | 3.3 | 3.3 | 3.3 | −5 |
Caphapirin | 77 | 7.5 | 9.5 | 3.3 | 3.3 | 3.3 | −2 | |
Cefquinome | 76 | 7.5 | 9.7 | 3.3 | 3.3 | 3.3 | 11 | |
Cefacetrile | 76 | 8.9 | 11 | 3.3 | 3.3 | 3.3 | −28 | |
Cefalonium | 75 | 6.8 | 8.8 | 3.3 | 3.3 | 3.3 | −9 | |
Cefalexin | 64 | 9.8 | 13 | 3.3 | 3.3 | 3.3 | 1 | |
Cefazolin b | 75 | 7.7 | 9.5 | 10 | 3.3 | 10 | 12 | |
Cefoperazone | 78 | 8.7 | 10 | 3.3 | 3.3 | 3.3 | −12 | |
Ceftiofur | 67 | 9.0 | 13 | 3.3 | 3.3 | 3.3 | −13 | |
Trimethoprim | Diaminopyrimidines | 77 | 9.8 | 11 | 3.3 | 3.3 | 3.3 | −7 |
Lincomycin | Lincosamides | 73 | 9.2 | 11 | 59 | 3.3 | 3.3 | −12 |
Pirlimycin | 60 | 14 | 14 | 3.3 | 3.3 | 3.3 | −11 | |
Tildipirosin | Macrolides | 63 | 8.3 | 11 | 3.3 | 3.3 | 3.3 | −2 |
Tulatromycin marker (CP 60,300) | 66 | 7.6 | 10 | 3.3 | 3.3 | 3.3 | −5 | |
Tulathromycin A b | 62 | 8.3 | 9.6 | 3.3 | 3.3 | 10 | −4 | |
Neospiramycin | 68 | 8.4 | 13 | 3.3 | 3.3 | 3.3 | −14 | |
Spiramycin I | 75 | 8.7 | 11 | 3.3 | 3.3 | 3.3 | −10 | |
Gamitromycin | 74 | 14 | 15 | 3.3 | 3.3 | 3.3 | −8 | |
Tilmicosin | 77 | 11 | 13 | 3.3 | 3.3 | 3.3 | −6 | |
Tylosin A | 82 | 10 | 13 | 242 | 3.3 | 3.3 | −10 | |
Erythromycin A | 80 | 7.3 | 10 | 175 | 3.3 | 3.3 | −12 | |
Tylosin-3-acetate | 85 | 11 | 13 | 244 | 3.3 | 3.3 | −4 | |
Tylvalosin | 90 | 9.5 | 14 | 245 | 3.3 | 3.3 | 17 | |
Amoxicillin | Penicillins | 65 | 8.2 | 11 | 3.3 | 3.3 | 3.3 | −5 |
Ampicillin | 69 | 7.8 | 9.7 | 3.3 | 3.3 | 3.3 | 1 | |
Penicillin G | 77 | 9.9 | 13 | 3.3 | 3.3 | 3.3 | −9 | |
Oxacillin | 77 | 8.8 | 9.8 | 3.3 | 3.3 | 3.3 | −9 | |
Penicillin V | 76 | 9.1 | 10 | 29 | 3.3 | 3.3 | −7 | |
Cloxacillin | 75 | 10 | 11 | 3.3 | 3.3 | 3.3 | −8 | |
Dicloxacillin | 74 | 9.1 | 11 | 3.3 | 3.3 | 3.3 | −18 | |
Nafcillin | 76 | 9.9 | 10 | 3.3 | 3.3 | 3.3 | −9 | |
Tiamulin | Pleuromutilins | 79 | 10 | 12 | 1199 | 3.3 | 3.3 | −18 |
Valnemulin | 76 | 9.8 | 15 | 3.3 | 3.3 | 3.3 | −40 | |
Marbofloxacin | Quinolones | 80 | 10 | 13 | 3.3 | 3.3 | 3.3 | −13 |
Norfloxacin | 69 | 7.4 | 13 | 3.3 | 3.3 | 3.3 | −12 | |
Enrofloxacin | 81 | 8.0 | 7.2 | 3.3 | 3.3 | 3.3 | −7 | |
Ciprofloxacin | 70 | 7.3 | 13 | 3.3 | 3.3 | 3.3 | −9 | |
Danofloxacin | 76 | 8.8 | 12 | 3.3 | 3.3 | 3.3 | 10 | |
Difloxacin | 81 | 9.4 | 11 | 3.3 | 3.3 | 3.3 | −2 | |
Sarafloxacin | 75 | 8.9 | 12 | 3.3 | 3.3 | 3.3 | −7 | |
Oxolinic acid | 82 | 8.6 | 11 | 3.3 | 3.3 | 3.3 | −13 | |
Nalidixic acid | 81 | 8.4 | 11 | 3.3 | 3.3 | 3.3 | −5 | |
Flumequine | 82 | 9.1 | 10 | 3.3 | 3.3 | 3.3 | −23 | |
Rifaximin | Rifamycins | 84 | 7.9 | 13 | 3.3 | 3.3 | 3.3 | 6 |
Sulfaguanidine | Sulfonamides | 76 | 8.8 | 12 | 3.3 | 3.3 | 3.3 | 20 |
Sulfanilamide | 76 | 8.3 | 11 | 3.3 | 3.3 | 3.3 | −7 | |
Sulfacetamide b | 76 | 7.3 | 8.1 | 10 | 3.3 | 10 | −1 | |
Sulfadiazine | 78 | 8.1 | 10 | 3.3 | 3.3 | 3.3 | 8 | |
Sulfathiazole | 78 | 7.8 | 9.2 | 3.3 | 3.3 | 3.3 | −9 | |
Sulfapyridine | 79 | 8.1 | 9.3 | 3.3 | 3.3 | 3.3 | −5 | |
Sulfamerazine b | 76 | 9.0 | 9.9 | 10 | 3.3 | 10 | 22 | |
Sulfamoxole | 76 | 7.9 | 11 | 3.3 | 3.3 | 3.3 | −12 | |
Sulfameter | 83 | 9.3 | 9.7 | 3.3 | 3.3 | 3.3 | −12 | |
Sulfamethizole | 78 | 8.4 | 10 | 3.3 | 3.3 | 3.3 | −3 | |
Sulfamethazine | 80 | 9.4 | 12 | 3.3 | 3.3 | 3.3 | −3 | |
Sulfamethoxypyridazine | 78 | 9.8 | 12 | 3.3 | 3.3 | 3.3 | −6 | |
Sulfachloropyridazine | 78 | 9.1 | 11 | 3.3 | 3.3 | 3.3 | −1 | |
Sulfamethoxazole | 81 | 8.6 | 10 | 3.3 | 3.3 | 3.3 | −14 | |
Sulfamonomethoxine | 80 | 9.2 | 11 | 3.3 | 3.3 | 3.3 | −3 | |
Sulfadoxin | 80 | 8.6 | 11 | 3.3 | 3.3 | 3.3 | −12 | |
Sulfisoxazole | 79 | 8.1 | 11 | 3.3 | 3.3 | 3.3 | −2 | |
Sulfadimethoxine | 81 | 7.9 | 9.9 | 3.3 | 3.3 | 3.3 | −22 | |
Sulfaquinoxaline | 80 | 7.7 | 10 | 3.3 | 3.3 | 3.3 | −25 | |
4-Epitetracycline | Tetracyclines | 68 | 7.7 | 9.2 | 230 | 3.3 | 3.3 | −5 |
4-Epioxytetracycline | 64 | 7.1 | 9.0 | 230 | 3.3 | 3.3 | 3 | |
Tetracycline | 72 | 8.0 | 11 | 235 | 3.3 | 3.3 | −1 | |
Oxytetracycline | 68 | 6.9 | 10 | 234 | 3.3 | 3.3 | 4 | |
4-Epichlortetracycline | 67 | 6.8 | 11 | 236 | 3.3 | 3.3 | 18 | |
Chlortetracycline | 73 | 6.3 | 10 | 233 | 3.3 | 3.3 | 16 | |
Doxycycline | 69 | 9.5 | 13 | 3.3 | 3.3 | 3.3 | −12 |
Detected Analyte | Detected Concentration (μg kg−1) | MRL (μg kg−1) | ADI (μg kg−1 b.w.) | ADI % (Mean) | ADI % (99th) | ||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Infants | Children | Teenagers | Adults | Elderly | Infants | Children | Teenagers | Adults | Elderly | ||||||||||
M | F | M | F | M | F | M | F | M | F | M | F | ||||||||
Doxycycline | 22 | Not fixed | 3 | 0.4 | 0.6 | 0.3 | 0.3 | 0.2 | 0.2 | 0.2 | 0.2 | 2.9 | 3.6 | 1.5 | 1.7 | 1.2 | 1.1 | 1.1 | 0.8 |
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Saluti, G.; Colagrande, M.N.; Castellani, F.; Ricci, M.; Diletti, G.; Scortichini, G. Survey on Antibiotic Residues in Egg Samples in Italy. Separations 2021, 8, 148. https://doi.org/10.3390/separations8090148
Saluti G, Colagrande MN, Castellani F, Ricci M, Diletti G, Scortichini G. Survey on Antibiotic Residues in Egg Samples in Italy. Separations. 2021; 8(9):148. https://doi.org/10.3390/separations8090148
Chicago/Turabian StyleSaluti, Giorgio, Maria Novella Colagrande, Federica Castellani, Matteo Ricci, Gianfranco Diletti, and Giampiero Scortichini. 2021. "Survey on Antibiotic Residues in Egg Samples in Italy" Separations 8, no. 9: 148. https://doi.org/10.3390/separations8090148