title: High-performance liquid chromatographic determination of spectinomycin in swine, calf and chicken plasma.
abstract: A rapid clean-up procedure based on ion-pair solid-phase extraction (SPE) for the high-performance liquid chromatographic (HPLC) determination of spectinomycin in swine, calf and chicken plasma at a limit of detection of 50 ng/ml is described. After dilution with water and adjustment of the pH to approximately 5.6, the plasma is applied to a high-hydrophobic C18 SPE column treated with sodium dioctylsulphosuccinate. Spectinomycin is eluted with methanol and derivatized with 2-naphthalene sulphonyl chloride prior to chromatography. The HPLC set-up consists of a dual-column system using two Chromspher silica columns and dichloromethane-acetonitrile-ethyl acetate-acetic acid, in different ratios, as mobile phases. Detection is performed at 250 nm. Quantification is carried out using external standards prepared in blank cleaned plasma. Mean recoveries were 83 +/- 3% (n = 5), 93 +/- 6% (n = 5) and 92 +/- 6% (n = 6) for swine, calf and chicken plasma, respectively, at the 0.1 microgram/ml level.
authors.affiliation: Department of the Science of Food and Animal Origin, Faculty of Veterinary Medicine, University of Utrecht, Netherlands.
authors.forename: N
authors.initials: N
authors.lastname: Haagsma
authors.forename: J R
authors.initials: JR
authors.lastname: Keegstra
authors.forename: P
authors.initials: P
authors.lastname: Scherpenisse
mesh_terms: D000818:Animals; D002417:Cattle; D002645:Chickens; D002851:Chromatography, High Pressure Liquid; D007202:Indicators and Reagents; D000198:Spectinomycin / Q000097:blood*; D013056:Spectrophotometry, Ultraviolet; D013552:Swine
chemical_list: D007202:Indicators and Reagents; D000198:Spectinomycin