Peyrovi Moazameh, Hadjmohammadi Mohammadreza
Department of Chemistry, University of Mazandran, Niroo-Havayii Boulevard, 47416-95447, Babolsar, Iran.
Biomed Chromatogr. 2015 Nov;29(11):1623-8. doi: 10.1002/bmc.3469. Epub 2015 Apr 14.
The aim of this work was to develop a method for the clean-up and preconcentration of warfarin from biological sample employing a new molecularly imprinted polymer (MIP) as a selective adsorbent for solid-phase extraction (SPE). This MIP was synthesized using warfarin as a template, pyrrole as a functional monomer and vinyl triethoxysilane as a cross-linker. The molar ratio of 1:4:20 (template-functional monomer-cross-linker) showed the best results. Nonimprinted polymers (NIPs) were prepared and treated with the same method, but in the absence of warfarin. The prepared polymer was characterized by Fourier transmission infrared spectrometry and scanning electron microscopy. An adsorption process (SPE) for the removal of warfarin using the fabricated MIPs and NIPs was evaluated under various conditions. Effective parameters on warfarin extraction, for example, type and volume of elution solvent, pH of sample solution, breakthrough volume and maximum loading capacity, were studied. The limits of detection were in the range of 0.0035-0.0050 µg mL(-1). Linearity of the method was determined in the range of 0.0165-10.0000 µg mL(-1) for plasma and 0.0115-10.0000 µg mL(-1) for urine with coefficients of determination (R(2)) ranging from 0.9975 to 0.9985. The recoveries for plasma and urine samples were >95%.
本研究旨在开发一种利用新型分子印迹聚合物（MIP）作为固相萃取（SPE）选择性吸附剂，从生物样品中净化和预富集华法林的方法。该MIP以华法林为模板、吡咯为功能单体、乙烯基三乙氧基硅烷为交联剂合成。1:4:20（模板-功能单体-交联剂）的摩尔比显示出最佳效果。制备了非印迹聚合物（NIP），并采用相同方法处理，但未使用华法林。通过傅里叶变换红外光谱和扫描电子显微镜对制备的聚合物进行了表征。在各种条件下评估了使用制备的MIP和NIP去除华法林的吸附过程（SPE）。研究了对华法林萃取的有效参数，如洗脱溶剂的类型和体积、样品溶液的pH值、穿透体积和最大负载量。检测限在0.0035 - 0.0050μg mL⁻¹范围内。该方法在血浆中的线性范围为0.0165 - 10.0000μg mL⁻¹，在尿液中的线性范围为0.0115 - 10.0000μg mL⁻¹，测定系数（R²）在0.9975至0.9985之间。血浆和尿液样品的回收率>95%。
