Colchicine is a naturally occurring alkaloid used in human and veterinary medicine. It shows genotoxicity in in vitro and in vivo systems even at low concentrations. Therefore, no ADI has been established, and colchicine has been included in Annex IV of Council Regulation (EEC) No. 2377/90. No abuse of this drug in intensive livestock farming has yet been reported. However, there may be a natural route of entry for this compound into the food chain when Colchicum autumnale is consumed by animals kept outdoors. To address this concern, we developed and validated a highly sensitive and selective quantitative LC-ESI-MS-MS method for the detection of colchicine in sheep serum and milk. For sample pretreatment, all samples were liquid-liquid extracted with phosphate buffer (pH 8.0) and dichloromethane. LC separation was carried out on an RP C18 column employing a 0.5% formic acid/acetonitrile gradient system. The recoveries in both matrixes at a concentration range from 0.0005 to 1 mg/L were >80% with RSDs of <10%. The applicability of the method was demonstrated in serum and the corresponding milk samples from Albanian sheep. After exposure to C. autumnale, the animals showed clinical signs of intoxication. Significant concentrations (up to 1 mg/L) of the drug were found in serum as well as in milk samples.

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The penetration of propoxur and phoxim from eggshell into whole egg was investigated in vitro by spraying eggs directly and in vivo after application of the compounds in henhouses. Although mean concentrations of the compounds on eggshells were up to 23000 microg kg(-1), mean residue concentrations in whole eggs were far below the current maximum residue levels (50 microg kg(-1) for propoxur and 60 microg kg(-1) for phoxim). These results provide the first evidence that propoxur and phoxim do not penetrate from eggshell into whole egg under experimental and field conditions. Subsequently, residue carry-over after egg cracking in households and during a worst-case situation in an egg-cracking plant was investigated. However, when eggs were cracked manually, a negligible contamination of whole egg values occurred. If, in an automated process, eggshells accidentally come into close contact with whole egg, very high residue levels of propoxur and phoxim may be generated time dependently. These results suggest that eggshell contact with whole egg during egg cracking must be avoided to prevent pesticide carry-over.