Preparation of Monolithic Imprinted Stationary Phase for Clenbuterol by In Situ Polymerization and Application in Biological Samples Pretreatment

Preparation of Monolithic Imprinted Stationary Phase for Clenbuterol by In Situ Polymerization and Application in Biological Samples Pretreatment
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原位聚合制备克伦特罗整体印迹固定相及其在生物样品前处理中的应用

DOI:
10.1007/s10337-011-2129-9
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发表时间:
2011-11-01
期刊:
影响因子:
1.7
通讯作者:
Chang, Chun
Chang, Chun
中科院分区:
化学4区
文献类型:
--
作者:
Luo, Yifen;Huang, Ping;Chang, Chun

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以甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,低极性溶剂(甲苯和十二醇)为致孔剂,采用原位聚合技术制备了对克伦特罗(CLB)等β 2-肾上腺素能受体激动剂具有特异识别作用的分子印迹整体固定相(MIMSP)。最佳聚合条件为:模板剂:单体:引发剂的摩尔比为5:20:1,EDMA占单体和EDMA总体积的85%(v/v),甲苯占总致孔剂的18%(v/v)。采用高效液相色谱法评价了该固定相对CLB和其他β(2)-肾上腺素能受体激动剂的选择性。采用Scatchard分析探讨了识别机理。以CLB-MIMSP为固相萃取固定相,对猪肝样品中的CLB进行富集和纯化。结果表明,所制备的CLB-MIMSP对CLB具有高度的选择性,对其他β 2-肾上腺素能受体激动剂具有中等的选择性,且具有制备简单的特点。方法的检出限为10 ng g(-1),加标回收率为99.16-113.06%,相对标准偏差为4.55-11.81%。CLB-MIMSP有望成为CLB生物样品预处理的理想固相萃取吸附剂。
A clenbuterol (CLB) molecule-imprinted monolithic stationary phase (MIMSP) with specific recognition for CLB and some other beta(2)-adrenergic receptor agonists was prepared by in situ polymerization technique utilizing methacrylic acid as a functional monomer, ethylene glycol dimethacrylate (EDMA) as a cross-linking reagent, and low polar solvents (toluene and dodecanol) as porogenic solvents. The optimal polymerization conditions were as follows: the molar ratio of template: monomer: initiator was 5:20:1, EDMA was 85% (v/v) in the total volume of monomer and EDMA, and toluene was 18% (v/v) in the total mixed porogen. The selectivity of the stationary phase for CLB and other beta(2)-adrenergic receptor agonists was evaluated by high performance liquid chromatography. Scatchard analysis was employed to explore the recognition mechanism. Then the CLB-MIMSP was used as a solid phase extraction (SPE) stationary phase for concentration and purification of CLB from pig liver samples. The results showed that the obtained CLB-MIMSP possessed high selectivity towards CLB and moderate selectivity towards some other beta(2)-adrenergic receptor agonists with characteristics of easy-made. The limit of detection was 10 ng g(-1), and recoveries of CLB were 99.16-113.06% with RSD 4.55-11.81% for the spiked pig liver samples. The CLB-MIMSP could be a promising SPE absorbent in CLB biological sample pretreatment.