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Maria Nobile UNIVERSITÀ DEGLI STUDI DI MILANO School of Veterinary Medicine PhD course in Veterinary and Animal Sciences Class XXX Development and validation of methods for the detection of residues in unconventional and innovative matrices through LC-MS/MS analyses for safety of food of animal origin. Maria Nobile Tutor: Prof. Luca Maria Chiesa Coordinator: Prof. Fulvio Gandolfi ACADEMIC YEAR 2016/2017 1 "Foodstuffs become blood; blood becomes heart and brain, the stuff of thought and attitudes. Human fare is the basis of human culture and thought. If you want to improve the people give it, instead of declamations against sin, better food. Man is what he eats." Ludwig A. Feuerbach 2 TABLE OF CONTENTS ABSTRACT .......................................................................................................... 5 CHAPTER 1 ............................................................................................................ 7 INTRODUCTION ....................................................................................................... 8 1.1. FOOD SAFETY AND ANALYSIS OF RESIDUES ...................................................... 8 1.2. THE USE OF VETERINARY DRUGS IN BREEDING ................................................. 9 1.3 CORTICOSTEROIDS: BIOSYNTHESIS, REGULATION AND METABOLISM ................ 12 1.3.1. Therapeutic use of corticosteroids in breeding ............................... 16 1.3.2. The prednisolone case: pseudoendogenous or illicit treatment? .... 17 1.3.3. Corticosteroids and legislations ...................................................... 18 1.3.4. Analytical approaches for corticosteroids ........................................ 20 1.4 ANABOLIC STEROIDS: BIOSYNTHESIS, REGULATION AND METABOLISM............... 21 1.4.1. Therapeutic use of anabolic steroids in breeding ............................ 23 1.4.2. Boldenone: another noteworthy case ............................................. 24 1.4.3. Anabolic steroids and legislations ................................................... 26 1.4.4. Analytical approaches for anabolic steroids .................................... 26 1.5 ANTIBIOTICS: GENERAL ASPECTS, SYNTHESIS AND MECHANISMS OF ACTION ..... 28 1.4.1. Antibiotic classes ........................................................................... .31 1.4.2. Therapeutic use of antibiotics in breeding ...................................... 42 1.4.3. Antibiotic resistance ........................................................................ 43 1.4.4. Antibiotics and legislation ............................................................... 46 1.4.5. Analytical approaches for antibiotics .............................................. 49 1.6 ENVIRONMENTAL CONTAMINATION AND EMERGENT POLLUTANT IN FOOD CHAIN . 51 1.7 PERFLUOROALKYL SUBSTANCES: GENERAL ASPECTS ..................................... 52 1.7.1. Perfluoroalkyl substances and legislations ..................................... 55 1.7.2. Analytical approaches for perfluoroalkyl substances ...................... 56 References ................................................................................................... 59 CHAPTER 2 .......................................................................................................... 75 2. AIMS ................................................................................................................ 76 References ................................................................................................... 79 CHAPTER 3 .......................................................................................................... 81 3. RESEARCH PAPERS ........................................................................................... 81 3.1. DETECTION OF BOLDENONE, ITS CONJUGATES AND ANDROSTADIENEDIONE, AS WELL AS FIVE CORTICOSTEROIDS IN BOVINE BILE THROUGH A UNIQUE IMMUNOAFFINITY COLUMN CLEAN-UP AND TWO VALIDATED LIQUID CHROMATOGRAPHY–TANDEM MASS SPECTROMETRY ANALYSES ...................... 82 3.2. SUITABILITY OF BOVINE BILE COMPARED TO URINE FOR DETECTION OF FREE, SULFATE AND GLUCURONATE BOLDENONE, ANDROSTADIENEDIONE, CORTISOL, 3 CORTISONE, PREDNISOLONE, PREDNISONE AND DEXAMETHASONE BY LC- MS/MS .................................................................................................... 104 3.3 DETECTION OF SELECTED CORTICOSTEROIDS AND ANABOLIC STEROIDS IN CALF MILK REPLACERS BY LIQUID CHROMATOGRAPHY–ELECTROSPRAY IONISATION – TANDEM MASS SPECTROMETRY ................................................................ 125 3.4. BOVINE TEETH AS A NOVEL MATRIX FOR THE CONTROL OF FOOD CHAIN: LIQUID CHROMATOGRAPHY–TANDEM MASS SPECTROMETRY DETECTION OF TREATMENTS WITH PREDNISOLONE, DEXAMETHASONE, ESTRADIOL, NANDROLONE AND SEVEN Β2-AGONISTS ....................................................... 147 3.5. DETERMINATION OF ENDOGENOUS AND EXOGENOUS CORTICOSTEROIDS IN BOVINE URINE AND EFFECT OF FIGHTING STRESS DURING THE “BATAILLES DES REINES” ON THEIR BIOSYNTHESIS ............................................................... 168 3.6. DETERMINATION OF VETERINARY ANTIBIOTICS IN BOVINE URINE BY LIQUID CHROMATOGRAPHY–TANDEM MASS SPECTROMETRY .................................... 190 3.7. A LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY METHOD FOR THE DETECTION OF ANTIMICROBIAL AGENTS FROM SEVEN CLASSES IN CALF MILK REPLACERS: VALIDATION AND APPLICATION ........................................ 217 3.8. ANTIBIOTIC USE IN HEAVY PIGS: COMPARISON BETWEEN URINE AND MUSCLE SAMPLES FROM FOOD CHAIN ANIMALS ANALYSED BY HPLC-MS/MS .............. 236 3.9. OCCURRENCE OF ANTIBIOTICS IN MUSSELS AND CLAMS FROM VARIOUS FAO AREAS ...................................................................................................... 258 3.10. DETECTION OF PERFLUOROALKYL ACIDS AND SULPHONATES IN ITALIAN EEL SAMPLES BY HPLC-HRMS ORBITRAP ....................................................... 278 3.11. FOOD SAFETY TRAITS OF MUSSELS AND CLAMS: DISTRIBUTION OF PCBS, PBDES, OCPS, PAHS AND PFASS IN SAMPLE FROM DIFFERENT AREAS USING HRMS-ORBITRAP® AND MODIFIED QUECHERS EXTRACTION FOLLOWED BY GC-MS/MS ........................................................................ 298 3.12. UNRAVELING ESTRADIOL METABOLISM AND INVOLVEMENT IN THE REPRODUCTIVE CYCLE OF NON VERTEBRATE ANIMALS: THE SEA URCHIN MODEL ..................................................................................................... 327 CHAPTER 4 ........................................................................................................ 362 4. CONCLUSIONS ................................................................................................ 363 4 ABSTRACT Successful animal growth depends on a combination of many factors related to health, management and nutrition. The use of veterinary drugs in food-producing animals for therapeutic purposes is regulated (corticosteroids, antibiotics) or banned (anabolic steroids) in the European Union; however, their use as growth promoters cannot be excluded. Moreover, the eventual presence of residues in food constitutes a fraud and a health issue for the consumers. For these reasons the need to find new accumulation matrices and new sensitive, specific and robust methods that are able to reveal the presence of drug residues is essential, based on the fact that there is a low percentage of non-conformity in the final reports of the National Residues Plan in recent years, although the threat of a disproportionate use of these substances is increasingly on the rise. In the light of these facts, there is the need to implement the framework of controls aimed to food safety, due to the inefficiency of tools for the study of these substances. Often, the use of conventional matrices, such as urine, liver or muscle, recommended for the official controls of illegal treatment are not completely satisfactory due to the fast elimination rate of the compounds or to the difficulties arising from the compounds characterised also by a pseudoendogenous nature. The debate about the presence of β-boldenone II phase metabolites and prednisolone in urine samples, owing to endogenous or illicit treatment, is currently ongoing within the European Union. These compounds have been appropriately defined “grey-zone substances”, for their double origin. The simple detection of some steroids in urine is currently considered to provide insufficient evidence of illicit treatment. Parameters such as cut-off levels, the presence of metabolites, or both, must be accounted for. As regards antibiotics, the overuse, over the last decades, as growth promoters in food producing animal have caused favorable condition about the threat of bacterial resistance. The antibiotics can directly affect the consumer in the form of residues from the food chain, or by accumulation in the environment via the application of manure to land as organic fertiliser, via sludge storage or by direct contamination of illicitly additivated water and feed. The main challenge is to monitor contemporally different antibiotic classes, in different steps of the food chain, trying to control this phenomenon. 5 On the other hand, food contamination by new environmental contaminants should not be neglected. In particular, perfluoroalkyl substances (PFASs) have recently aroused great scientific interest and concern for public health, due to the fact they have been found in appreciable concentrations in human serum. On the basis of EFSA requestes and of analytical problems associated with their determination many studies are recommended to
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