Gorbani Yagoup, Yılmaz Hüma, Basan Hasan
Department of Analytical Chemistry, Gazi University, Ankara, Turkey.
Luminescence. 2017 Dec;32(8):1391-1397. doi: 10.1002/bio.3335. Epub 2017 Jun 1.
This study presents a novel, sensitive and selective molecularly imprinted solid-phase extraction (MISPE)-spectrofluorimetric method for the removal and determination of atenolol from human urine. Molecularly imprinted and non-imprinted polymers were synthesized thermally using a radical chain polymerization technique and used as solid-phase extraction sorbents. Acrylic acid ethylene glycol dimethacrylate, dibenzoyl peroxide and dichloroethane were used as a functional monomer, cross-linker, initiator and porogen, respectively. The calibration curve was in the range of 0.10-2.0 μg/ml for the developed method. Limit of detection and limit of quantification values were 0.032 and 0.099 μg/ml, respectively. Owing to the selectivity of the MISPE technique and the sensitivity of spectrofluorimetry, trace levels of atenolol have been successfully determined from both organic and aqueous media. Relatively high imprinting factor (4.18) and recovery results (74.5-75.3%) were obtained. In addition, intra- and interday precision values were 0.38-1.03% and 0.47-2.05%, respectively, proving the precision of the proposed method. Thus, a selective, sensitive and simple MISPE-spectrofluorimetric method has been developed and applied to the direct determination of atenolol from human urine.
本研究提出了一种新颖、灵敏且具有选择性的分子印迹固相萃取（MISPE）-荧光光谱法，用于从人尿中去除和测定阿替洛尔。采用自由基链聚合法热合成了分子印迹聚合物和非印迹聚合物，并将其用作固相萃取吸附剂。丙烯酸、乙二醇二甲基丙烯酸酯、过氧化二苯甲酰和二氯乙烷分别用作功能单体、交联剂、引发剂和致孔剂。所开发方法的校准曲线范围为0.10 - 2.0μg/ml。检测限和定量限分别为0.032和0.099μg/ml。由于MISPE技术的选择性和荧光光谱法的灵敏度，已成功从有机介质和水介质中测定痕量水平的阿替洛尔。获得了相对较高的印迹因子（4.18）和回收率结果（74.5 - 75.3%）。此外，日内和日间精密度值分别为0.38 - 1.03%和0.47 - 2.05%，证明了所提方法的精密度。因此，已开发出一种选择性、灵敏且简单的MISPE - 荧光光谱法，并将其应用于直接测定人尿中的阿替洛尔。
