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On-line extraction and determination of residual sulfathiazole in pharmaceutical wastewater with molecularly imprinted polymers in a packed cartridge coupled with high-performance liquid chromatography

机译:用高性能液相色谱,分子印迹聚合物在填充筒中具有分子印迹聚合物的药物废水中残留磺唑唑的直线提取及测定

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摘要

A new, rapid and sensitive on-line extraction and determination technique was developed with molecularly imprinted polymers (MIPs) in a packed cartridge. An artificial selective polymeric sorbents packed in a polyethylene cartridge were employed for the separation of sulfathiazole residue. The packing particles were synthesized using methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker agent, sulfathiazole as a target template molecule and azobisisobutyronitrile as an initiator. The optimal conditions for designing these sorbents were as follows: conditioning using water with pH = 3.0, loading the sample under mild basic aqueous conditions, cleanup using 2 x 2 mL acetonitrile and elution with 3.0 mL 20 mM ammonium acetate : acetonitrile (75 : 25 v/v, pH = 3.0). In this system, an aliquot of extracted template was injected to the HPLC analytical column with acetonitrile : water (75 : 25 v/v) and water (pH adjusted to 3.0 with H3PO4) as the mobile phases in a gradient elution program. The selectivity of the MIPs in the packed cartridge was evaluated by checking several substances with molecular structures similar to that of the template. The results revealed a recovery of more than 92% along with a limit of detection and limit of quantification of 0.05 and 0.16 ng mL(-1), respectively, for the on-line determination of sulfathiazole in pharmaceutical wastewater samples.
机译:在包装盒中使用分子印迹聚合物(MIPS)开发了一种新的,快速灵敏的在线提取和测定技术。用填充在聚乙烯盒中的人造选择性聚合物吸附剂用于分离磺胺唑烷残余物。使用甲基丙烯酸作为官能单体,乙二醇二甲基丙烯酸酯作为交联剂,作为靶模板分子和偶氮二异丁腈作为引发剂的乙二醇。用于设计这些吸附剂的最佳条件如下:使用水的水调节pH = 3.0,在温和的碱性条件下加载样品,使用2×2ml乙腈清除,用3.0ml 20mM乙酸铵洗脱:乙腈(75:25 v / v,pH = 3.0)。在该系统中,用乙腈注射到HPLC分析柱中的等分试样:水(75:25V / v)和水(用H3PO4调节至3.0)作为梯度洗脱计划中的移动相。通过检查与模板类似的分子结构的几种物质来评估包装盒中的MIPS的选择性。结果显示出超过92%的回收率,并且分别具有0.05和0.16mL(-1)的量化限制,用于药物废水样品中的苏硫酸甲唑的在线测定。

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