Development and validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous determination of nine corticosteroid residues in bovine liver samples

A liquid chromatography tandem mass spectrometry (LC-MS/MS) confirmatory method for the simultaneous determination of nine corticosteroids in liver, including the four MRL compounds listed in Council Regulation 37/2010, was developed. After an enzymatic deconjugation and a solvent extraction of the liver tissue, the resulting solution was cleaned up through an SPE Oasis HLB cartridge. The analytes were then detected by liquid chromatography-negative-ion electrospray tandem mass spectrometry, using deuterium-labelled internal standards. The procedure was validated as a quantitative confirmatory method according to the Commission Decision 2002/657/EC criteria. The results showed that the method was suitable for statutory residue testing regarding the following performance characteristics: instrumental linearity, specificity, precision (repeatability and intra-laboratory reproducibility), recovery, decision limit (CCα), detection capability (CCβ) and ruggedness. All the corticosteroids can be detected at a concentration around 1 μg kg(-1); the recoveries were above 62% for all the analytes. Repeatability and reproducibility (within-laboratory reproducibility) for all the analytes were below 7.65% and 15.5%, respectively.

Lutetia׳s lineaments

The European Space Agency׳s Rosetta spacecraft flew by asteroid (21) Lutetia on July 10, 2010. Observations through the OSIRIS camera have revealed many geological features. Lineaments are identified on the entire observed surface of the asteroid. Many of these features are concentric around the North Pole Crater Cluster (NPCC). As observed on (433) Eros and (4) Vesta, this analysis of Lutetia assesses whether or not some of the lineaments could be created orthogonally to observed impact craters. The results indicate that the orientation of lineaments on Lutetia׳s surface could be explained by three impact craters: the Massilia and the NPCC craters observed in the northern hemisphere, and candidate crater Suspicio inferred to be in the southern hemisphere. The latter has not been observed during the Rosetta flyby. Of note, is that the inferred location of the Suspicio impact crater derived from lineaments matches locations where hydrated minerals have been detected from Earth-based observations in the southern hemisphere of Lutetia. Although the presence of these minerals has to be confirmed, this analysis shows that the topography may also have a significant contribution in the modification of the spectral shape and its interpretation. The cross-cutting relationships of craters with lineaments, or between lineaments themselves show that Massilia is the oldest of the three impact feature, the NPCC the youngest, and that the Suspicio impact crater is of intermediate age that is likely occurred closer in time to the Massilia event.