High-performance liquid chromatographic assay for the determination of a semisynthetic avermectin analog (eprinomectin) in bovine milk at parts per billion levels—method development and validation

A sensitive and automated method has been developed and validated to determine marker residue eprinomectin B 1a in bovine milk. Extraction of eprinomectin B 1a from milk is accomplished with acetonitrile after the addition of an internal standard. The extract containing the analytes is evaporated to...

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Veröffentlicht in:Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2002-05, Vol.772 (1), p.99-105
Hauptverfasser: Pollmeier, M., Maier, S., Moriarty, K., DeMontigny, P.
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Sprache:eng
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Zusammenfassung:A sensitive and automated method has been developed and validated to determine marker residue eprinomectin B 1a in bovine milk. Extraction of eprinomectin B 1a from milk is accomplished with acetonitrile after the addition of an internal standard. The extract containing the analytes is evaporated to dryness and reconstituted in a solution containing 30% 1- N-methylimidazole in acetonitrile. Online derivatization is carried out with trifluoroacetic anhydride. Determination of eprinomectin B 1a and its internal standard is carried out by HPLC using a reversed-phase C 18 column with a mobile phase consisting of methanol, acetonitrile, water, triethylamine and phosphoric acid. The overall extraction recovery of eprinomectin B 1a is 94% with milk supplemented between 2 and 50 ng/ml eprinomectin B 1a. Precision RSD averaged 3.0% in Laboratory 1 ( n=25) compared to 4.3% in Laboratory 2 ( n=35). The limit of quantitation is approximately 2 ng/ml eprinomectin B 1a, the limit of detection is approximately 0.25 ng/ml using this method.
ISSN:1570-0232
1873-376X
DOI:10.1016/S1570-0232(02)00063-6