Department of Chemistry, Amirkabir University of Technology, Tehran, Iran.
J Mater Sci Mater Med. 2012 Jun;23(6):1543-52. doi: 10.1007/s10856-012-4623-5. Epub 2012 Apr 7.
This paper describes a new method for the determination of citalopram in biological fluids using molecularly imprinted solid-phase extraction as the sample cleanup technique combined with high performance liquid chromatography. The molecularly imprinted polymers were prepared using methacrylic acid as functional monomer, ethylene glycol dimethacrylate as crosslinker, chloroform as porogen and citalopram hydrobromide as the template molecule. The novel imprinted polymer was used as a solid-phase extraction sorbent for the extraction of citalopram from human serum and urine. Effective parameters on citalopram retention were studied. The optimal conditions for molecularly imprinted solid-phase extraction consisted of conditioning with 1 mL methanol and 1 mL of deionized water at neutral pH, loading of citalopram sample (50 μg L(-1)) at pH 9.0, washing using 1 mL acetone and elution with 3 × 1 mL of 10 % (v/v) acetic acid in methanol. The MIP selectivity was evaluated by checking several substances with similar molecular structures to that of citalopram. Results from the HPLC analyses showed that the calibration curve of citalopram using MIP from human serum and urine is linear in the ranges of 1-100 and 2-120 μg L(-1) with good precisions (2.5 and 1.5 % for 10.0 μg L(-1)), and recoveries (between 82-86 and 83-85 %), respectively.
本文描述了一种新的方法，用于使用分子印迹固相萃取作为样品净化技术，结合高效液相色谱法，测定生物流体中的西酞普兰。分子印迹聚合物是用甲基丙烯酸作为功能单体、乙二醇二甲基丙烯酸酯作为交联剂、氯仿作为致孔剂和氢溴酸西酞普兰作为模板分子制备的。新型印迹聚合物被用作固相萃取吸附剂，从人血清和尿液中提取西酞普兰。研究了影响西酞普兰保留的有效参数。分子印迹固相萃取的最佳条件为：中性 pH 值下用 1 mL 甲醇和 1 mL 去离子水进行预处理，在 pH 9.0 下加载 50 μg L(-1)的西酞普兰样品，用 1 mL 丙酮洗涤，用 3 × 1 mL 10%（v/v）甲醇中的乙酸洗脱。通过检查几种与西酞普兰具有相似分子结构的物质来评估 MIP 的选择性。高效液相色谱分析结果表明，使用来自人血清和尿液的 MIP 测定西酞普兰的校准曲线在 1-100 和 2-120 μg L(-1)范围内具有良好的线性，精密度良好（10.0 μg L(-1)时为 2.5%和 1.5%），回收率分别为 82-86%和 83-85%。
