| Autor: |
Hornish RE; Pharmacia and Upjohn Worldwide Animal Health, Kalamazoo, MI 49001, USA., Wiest JR |
| Jazyk: |
angličtina |
| Zdroj: |
Journal of chromatography. A [J Chromatogr A] 1998 Jul 03; Vol. 812 (1-2), pp. 123-33. |
| DOI: |
10.1016/s0021-9673(98)00368-9 |
| Abstrakt: |
Determinative and confirmatory methods of analysis for spectinomycin residue in bovine kidney, liver, muscle and fat have been developed. The determinative method is a single-column HPLC ion-exchange procedure that incorporates a two-step post-column oxidation of the secondary amines to primary amines followed by derivatization with o-phthalaldehyde. The method was validated in all tissues to a low-end concentration of 0.10 micrograms/g (limit of quantitation) and to a high-end of 10 micrograms/g for kidney, which is the rate-limiting tissue for residues of spectinomycin. The recovery of spectinomycin from all tissues was > 80% and the variability (R.S.D.) was generally < 10%. For liver, an alternative reversed-phase HPLC separation was required for incurred-residue samples. The confirmatory method employed an atmospheric pressure chemical ionization-MS-MS approach utilizing a rapid reversed-phase HPLC system with a mobile phase of methanol and 1% acetic acid. The protonated molecular ion for spectinomycin at m/z 333 produced four diagnostic reaction-product ions at 98, 116, 158 and 189 for confirmation. The method was validated to a lower limit of confirmation of 0.10 micrograms/g. |
| Databáze: |
MEDLINE |
| Externí odkaz: |
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