Journal
JOURNAL OF SEPARATION SCIENCE
Volume 38, Issue 21, Pages 3743-3749Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201500373
Keywords
Antibiotics; Macrolides; Milk; Quick, easy, cheap, effective, rugged, and safe; Residues
Categories
Funding
- Brazilian National Council for Scientific and Technological Development (CNPq)
- CNPq
- State of Rio de Janeiro Carlos Chagas Filho Research Foundation (Faperj)
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A simple extraction technique has been developed for seven macrolide antibiotics in milk. The procedure involves a modified quick, easy, cheap, effective, rugged, and safe method based on acetonitrile extraction, followed by the addition of a mixture of salts ( sodium sulfate, sodium chloride, and potassium carbonate) not yet reported in literature. The method was validated for tylosin and was selective, free of matrix effect, and linear in the range of 0.78-18.75 ng/mL in the final extract, corresponding to 0.125-3 times the maximum residue limit. The limit of detection, limit of quantification, decision limit, and detection capability were, respectively, 0.84, 2.79, 58.4, and 71.7 mu g/kg. The overall average recovery at 25, 50, and 75 mu g/kg ranged from 89-97%. Repeatability and intermediate precision expressed by relative standard deviations were below 10.5 and 12%, respectively. The extension of the validation for spiramycin, throleandomycin, oleandomycin, roxithromycin, erythromycin, and clarithromycin is under consideration since the procedure proved to be able to efficiently extract all studied macrolides, with recoveries from 74-104% at 50 mu g/kg for tylosin, erythromycin, spiramycin, and oleandomycin and 20 mu g/kg for throleandomycin, roxithromycin, and clarithromycin.
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