Journal of Separation Science 2011-02-01

Determination of cypromazine and its metabolite melamine in milk by cation-selective exhaustive injection and sweeping-capillary micellar electrokinetic chromatography.

Xuegang Li, Jiwei Hu, Heyou Han

Index: J. Sep. Sci. 34(3) , 323-30, (2011)

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Abstract

In this study, we described a high-sensitive on-line preconcentration method for cypromazine (CYP) and melamine (MEL) analysis using cation-selective exhaustive injection (CSEI) combined with sweeping-MEKC. The optimum conditions of on-line concentration and separation were discussed. The BGE contained 100 mM SDS, 50 mM phosphoric acid (pH=2.0) and 15% acetonitrile (v/v). The sample was injected at 10 kV for 600 s, separated at -20 kV, and detected at 210 nm. The sensitivity enhancements were 6222 for CYP and 9179 for MEL. The linear dynamic ranges were 0.4-25 ng/mL for CYP (r=0.9995) and 0.2-12 ng/mL for MEL (r=0.9991). The LODs (signal-to-noise ratio, 3) were 43.7 and 23.4 pg/mL for CYP and MEL, respectively. The proposed method was applied to analyze CYP and MEL in dairy products pretreated using off-line SPE to minimize the influence of the matrix. The recoveries of CYP and MEL were satisfactory (ca. 74-83%). The experimental results suggest that the CSEI-sweeping-MEKC method is feasible for the application to simultaneously detect trace levels of CYP and its metabolite MEL in real milk samples.Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.