Key Laboratory of Applied Technology of Marine Biology, Ministry of Education, Faculty of Life Science and Biotechnology, Ningbo University, Ningbo, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 May 1;879(15-16):1071-6. doi: 10.1016/j.jchromb.2011.03.019. Epub 2011 Mar 16.
Group-selective molecularly imprinted polymers (MIPs) made from sulfonamides (SAs) using functional monomer methacrylic acid (MAA) were synthesized. The derived molecularly imprinted solid-phase extraction (MISPE) cartridges were developed for the purification and enrichment of aquatic products. The optimum template molecule and the ratio of the functional monomer to the template for obtaining group selectivity to SAs were sulfadimethoxine (SDM) and 4:1, respectively. The MIPs were characterized by Brunauer-Emmett-Teller (BET), scatchard plot, and chromatography analysis, all of which demonstrate better chromatographic behavior and group-selectivity of MIPs for SAs compared with those of corresponding NIPs. The extraction conditions of MISPE for six SAs were optimized; the method precision and accuracy were satisfactory for the fish and shrimp samples at 0.05, 0.1, and 0.2 mg kg(-1) spiked levels. Recoveries ranging from 85.5% to 106.1% (RSD, 1.2-7.0%, n=3) were achieved. The limits of detection (S/N=3) and quantitation (S/N=10) in the shrimp and fish samples were achieved from 8.4 to 10.9 μg kg(-1) and from 22.4 to 27.7 μg kg(-1), respectively. Therefore, the obtained MIPs and MISPE can be employed for the enrichment and clean-up of SAs. This paper presents a new analytical method which enables the simultaneous determination and quantification of SAs in aquaculture products.
采用功能单体甲基丙烯酸(MAA)合成了磺胺类(SAs)的选择性分子印迹聚合物(MIPs)。开发了衍生的分子印迹固相萃取(MISPE)小柱,用于水产养殖产品的净化和富集。获得对 SAs 具有组选择性的最佳模板分子和功能单体与模板的比例分别为磺胺二甲氧嘧啶(SDM)和 4:1。通过 Brunauer-Emmett-Teller(BET)、Scatchard 图和色谱分析对 MIPs 进行了表征,所有这些都表明 MIPs 对 SAs 的色谱行为和组选择性均优于相应的 NIPs。优化了 MISPE 对六种 SAs 的萃取条件;该方法在 0.05、0.1 和 0.2 mg kg(-1) 加标水平的鱼和虾样品中的精密度和准确度均令人满意。回收率在 85.5%至 106.1%(RSD,1.2-7.0%,n=3)之间。虾和鱼样品中的检出限(S/N=3)和定量限(S/N=10)分别为 8.4 至 10.9 μg kg(-1)和 22.4 至 27.7 μg kg(-1)。因此,获得的 MIPs 和 MISPE 可用于 SAs 的富集和净化。本文提出了一种新的分析方法,可用于同时测定和定量水产养殖产品中的 SAs。