Abstract

A molecularly imprinted monolith was prepared and evaluated for the special selective separation of sulfamerazine (SMR) by capillary electrochromatography (CEC). The single-step in situ polymerization method was applied through thermally immobilized vinyl groups of itaconic acid and a derivatization capillary column using SMR as the template. The monolith with optimal selectivity and permeability was performed at 45°C for 7 h according to the molar ratios of 1 : 4 : 10 (template/functional monomer/cross-linker). Under the optimized separation conditions of 75% acetonitrile in 20 mM phosphate buffer with pH 5.0, 15 kV applied voltage and 20°C column temperature, the imprinted monolith showed strong recognition ability for SMR and high column performance. Finally, the molecularly imprinted monolith coupled with the CEC method was successfully developed for the quantification of SMR in aquatic products, which was properly validated by a good linear relationship, recoveries and limit of detection. The coupling technique of the molecularly imprinted technology and CEC achieved pre-treatment enrichment and separation analysis in only one miniaturized chromatographic column.

Highlights

  • Sulfonamides (SAs) were among the first synthetic antibiotics and are widely used in humans and animals, but there is significant concern about their negative impacts on the ecosystem and human health after use [1,2]

  • It is important to realize that the Capillary electrochromatography (CEC) system operates with small sample quantities and sample vials used for the introduction of the sample only require microlitre quantities, which is quite attractive for precious biological samples [7]

  • The resultant column performance was evaluated by the permeability and the ratio of the retention factor (I ) in which I 1⁄4 K1/K2, where K1 and K2 are the retention of SMR on the imprinted monolith and non-imprinted monolith, respectively, and K 1⁄4/t0, where tR and t0 are the migration time of the retained peak and non-retained neutral thiourea, respectively

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Summary

Introduction

Sulfonamides (SAs) were among the first synthetic antibiotics and are widely used in humans and animals, but there is significant concern about their negative impacts on the ecosystem and human health after use [1,2]. The efficient and accurate determination of trace SAs in some complex matrix samples is necessary for the testing organization. Several CEC studies on SA separations have been reported by Wang & Ye [8] and Krivohlavek et al [9]. In these cases, C18 packed columns were used to analyse SAs; long separation time or poor peak resolution was observed. The authors suggested using poly(divinylbenzene-octyl methacrylate) monolithic stationary phases for the successful detection of sulfamerazine (SMR) in meat samples using in-line solid phase extraction (SPE)-CEC with a mass spectrometry (MS) detector system. It is obvious that the development of a relevant stationary phase for the detection of SAs is necessary

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