[Fluorometric determination of sulfanilamide and sulfaguanidine residues in animal tissues with high-performance-liquid chromatography].
A high-performance liquid chromatographic method is presented for the selective analysis of sulphanilamide (SA) and sulphaguanidine (SG) residues in animal tissues (muscle, liver), egg and milk at the 0.01-0.1 mg/kg level. A 25-g amount of the samples was extracted with 90 ml acetonitrile at pH 8.5 to which 2 ml saturated sodium carbonate had been added. After centrifugation, co-extracted water was separated by saturating the extract with sodium chloride and adding 50 ml dichloromethane. The residue of the dried and evaporated organic layer was partitioned between methanol, n-hexane and mobile phase (1 ml each). A 20-microliter volume of the aqueous layer was injected onto a Nucleosil 5 SA column [mobile phase 0.05 M sodium dihydrogenphosphate (adjusted to pH 2.0 with 85% orthophosphoric acid)-methanol, 85:15, v/v]. SA and SG were detected by their native fluorescence (excitation 275 nm, emission 340 nm) at retention times of 7 and 13 min, respectively, without interference of co-extractives. Parallel detection by ultraviolet absorption (275 nm) allowed on-line confirmation of the results. Recovery of spiked samples (0.1 mg/kg) was 80% (coefficient of variation, C.V. = 5%) for SA and 62% (C.V. = 6%) for SG. Concentrations of 0.27 mg/kg for SA and 0.05 mg/kg for SG were analyzed in muscle meat of a swine which received a single intramuscular injection of 2.1 g SA and 0.6 g SG and was slaughtered 24 h later.
Institut für Lebensmittelchemie, Universität Münster, B.R.D.
M
M
Petz
D000818:Animals; D002417:Cattle; D002851:Chromatography, High Pressure Liquid; D004531:Eggs / Q000032:analysis; D006146:Guanidines / Q000032:analysis*; D006863:Hydrogen-Ion Concentration; D007202:Indicators and Reagents; D008892:Milk / Q000032:analysis; D013050:Spectrometry, Fluorescence; D013056:Spectrophotometry, Ultraviolet; D013414:Sulfaguanidine / Q000032:analysis*; D013424:Sulfanilamides / Q000032:analysis*; D013552:Swine
D006146:Guanidines; D007202:Indicators and Reagents; D013424:Sulfanilamides; D013414:Sulfaguanidine
Fluorimetrische Bestimmung von Sulfanilamid- und Sulfaguanidinrückständen in tierischen Matrices durch Ionenaustausch-Hochleistungsflüssig-chromatographie.