Confirmatory Method for the Determination of Streptomycin and Dihydrostreptomycin in Honey by LC-MS/MS
Bohm, Detlef A.
Stachel, Carolin S.
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Abstract The method was specifically developed for the determination and confirmation of streptomycin and dihydrostreptomycin in different types of honey. The method is simple, rapid, sensitive and was validated for streptomycin and dihydrostreptomycin in accordance with Commission.Decision 2002/657/EC. After extraction with phosphate buffer and a pH change, the clean-up was performed by way of SPE with polymeric phase. The LC-MS/MS analysis was carried out testing two different HILIC columns for the separation of the analytes and using a triple quadrupole mass spectrometer in positive ESI mode to measure the transitions of the substances in MRM mode. For the quantification of both substances matrix calibration curves in the linear range of 5 ? 80 ?g/kg were used. The calculated validation parameters for streptomycin and dihydrostreptomycin like CC? (11.8 and 11.5 ?g/kg), CC? (18.9 and 19.9 ?g/kg) and the recovery (97 and 101 %) respectively the relative within-laboratory reproducibility RSDwR (16.4 and 20.8 %) at the recommended concentration of 40 ?g/kg fulfil the requirements of Commission Decision 2002/657/EC. Keywords: streptomycin, dihydrostreptomycin, honey, LC-MS/MS, validation, CD 2002/657/EC, CC?, CC?
Publisher:Taylor & Francis
Affiliation:Federal Office of Consumer Protection and Food Safety, NRL for Contaminants and Residues - Mauerstr. 39-42--> - 10117 - Berlin - GERMANY (Bohm, Detlef A.)
Federal Office of Consumer Protection and Food Safety, NRL for Contaminants and Residues - Berlin - GERMANY (Stachel, Carolin S.)
Federal Office of Consumer Protection and Food Safety, NRL for Contaminants and Residues - Berlin - GERMANY (gowik, petra)