Rapid determination of sulphonamides in milk using liquid chromatographic separation and fluorescamine derivatization

Journal of Chromatography
N Takeda, Y Akiyama

Abstract

A simple and selective method is presented for the multiple residue determination of eight sulphonamides in consumers' milk. The drugs are sulphisomidine (ID), sulphadiazine (DZ), sulphamerazine, sulphadimidine, sulphamonomethoxine, sulphamethoxazole, sulphadimethoxine and sulphaquinoxaline (SQ). The milk sample was deproteinized with the same volume of 2 M hydrochloric acid and filtered. A 1-ml volume of the filtrate was mixed with 1 ml each of 1.25 M sodium acetate solution and a buffer (pH 3.0) for derivatization with 0.6 ml of 0.02% fluorescamine solution in acetone. A high-performance liquid chromatographic analysis was carried out on a C18 column with a mobile phase of acetonitrile-2% acetic acid (3:5) at 55 degrees C using a fluorescence detector at an excitation wavelength of 405 nm and an emission wavelength of 495 nm. Average recoveries at fortification levels of 2, 5 and 10 ng/ml were 114%, 109% and 106%, respectively. Relative standard deviations were 1-4% at 10 ng/ml for ID, 5 ng/ml for DZ and SQ and 2.5 ng/ml for the other five sulphonamides. The method was applied to 25 milk samples and all appeared to be free from the drugs.

Citations

Sep 1, 1994·Journal of Pharmaceutical and Biomedical Analysis·M C MahederoJ J Aaron
Mar 1, 1995·Journal of Pharmaceutical and Biomedical Analysis·M C García-Alvarez-CoqueJ S Esteve-Romero
Feb 17, 1998·Journal of Chromatography. a·C E LinS W Wang
May 15, 2002·Journal of Pharmaceutical and Biomedical Analysis·Nesrin CesurS Ozkirimli
Jul 11, 2008·Journal of Separation Science·Victoria Samanidou, Styliani Nisyriou
Jun 8, 1999·The Veterinary Record·J D McEvoyD G Kennedy

Related Concepts

Metazoa
Liquid Chromatography
Enzyme-Linked Immunosorbent Assay
Fluram
Indicators
Spectrophotometry, Ultraviolet
Sulfonamides

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