High performance liquid chromatography post-column chemiluminescence determination of sulfonamide residues in milk at low concentration levels using bis[4-nitro-2-(3,6,9-trioxadecyloxycarbonyl)phenyl] oxalate as chemiluminescent reagent.
The determination of seven sulfonamides by means of HPLC with chemiluminescence detection is proposed for the first time. The analytes are derivatized with fluorescamine, separated and subsequently they participate in the post-column chemiluminescence (CL) peroxyoxalate system using imidazole as a catalyst. Among the different peroxyoxalates tested, bis[4-nitro-2-(3,6,9-trioxadecyloxycarbonyl)phenyl] oxalate provides higher sensitivities and stabilities, avoiding precipitation problems. A rigorous optimization of the significant variables by means of experimental designs has been developed in order to reconcile the chromatographic conditions with the CL reaction. The method provides detection limits in the low microgl(-1) range and has been satisfactorily applied to the analysis of spiked raw milk samples.
Soto-Chinchilla
Jorge J
JJ
Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Spain.
Gámiz-Gracia
Laura
L
García-Campaña
Ana M
AM
Imai
Kazuhiro
K
García-Ayuso
Luis E
LE
D000818:Animals; D002138:Calibration; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005260:Female; D005450:Fluorescamine / Q000737:chemistry; D007202:Indicators and Reagents / Q000737:chemistry; D008163:Luminescent Measurements / Q000379:methods*; D008892:Milk / Q000737:chemistry*; D010070:Oxalates / Q000737:chemistry*; D012680:Sensitivity and Specificity; D013449:Sulfonamides / Q000032:analysis* / Q000737:chemistry
D007202:Indicators and Reagents; D010070:Oxalates; D013449:Sulfonamides; C054009:bis(4-nitro-2-(3,6,9-trioxadecyloxycarbonyl)phenyl)oxalate; D005450:Fluorescamine