Determination of 11 sulfonamide residues in aquaculture water and sediments by high performance liquid chromatography coupled with post-column derivatization

doi:10.3724/SP.J.1123.2014.12022

Abstract

Abstract:

An analytical method was developed for the determination of 11 sulfonamide compounds in aquaculture water and sediments by high performance liquid chromatography (HPLC) coupled with post-column derivatization. The filtered water sample was purified and concentrated with HLB cartridge, while the sediment sample was extracted with a mixture of methanol and EDTA-Mcllvaine buffer (1:1, v/v), and then purified and enriched through HLB solid-phase extraction. The sulfonamides were separated on a C₁₈ column by HPLC and on-line derivatized with a fluorescamine and detected with a fluorescence detector. The parameters of post-column derivatization system were optimized, and the fluorescamine solution concentration, velocity of reagent solution and reaction temperature were 0.2 g/L, 0.15 mL/min and 50 ℃, respectively. The calibration curves of the method showed good linearity in the range of 0.01-1.0 mg/L, with the correlation coefficients (r²) all above 0.99995. The recoveries were 79.3%-100.7% and 74.6%-95.3% with RSD values of 2.2%-11.0% and 2.6%-10.3% for the 11 sulfonamides in aquaculture water and sediments, respectively. The respective limits of detection (LODs, S/N=3) were 0.9-5.5 ng/L and 0.3-1.3 μg/kg and the limits of quantification (LOQs, S/N=10) were 3.0-18.1 ng/L and 1.0-4.4 μg/kg. The method can be applied to the determination of sulfonamides in the aquaculture environment, and it has a good practicability.

Key words: aquaculture water, high performance liquid chromatography (HPLC), post-column derivatization, sediments, sulfonamides (SAs)

CLC Number:

O658

LIU Jinghua, SUN Zhenzhong, HUANG Xueling, GUO Xia, SUN Jianhua. Determination of 11 sulfonamide residues in aquaculture water and sediments by high performance liquid chromatography coupled with post-column derivatization[J]. Chinese Journal of Chromatography, 2015, 33(4): 434-440.

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