Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran.
Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran.
J Pharm Biomed Anal. 2021 Sep 10;204:114256. doi: 10.1016/j.jpba.2021.114256. Epub 2021 Jul 13.
A nanocomposite of molecularly imprinted polypyrrole on copper oxide (MIP@CuO) was introduced as a new coating for in-tube solid-phase microextraction (IT-SPME). The method coupled with HPLC-UV was successfully applied for analysis of carbamazepine (anticonvulsant and bipolar disorder medication) in biological samples. First, in order to increase the surface area and stability of the coating, copper oxide (CuO) nanosheets were synthesized on the inner surface of a copper tube using a chemical method. Then, molecularly imprinted polypyrrole coating (using carbamazepine as a template) was deposited on CuO by a facile in-situ electrodeposition method. According to the results, The MIP@CuO coating shows long life time, enhanced extraction efficiency, and good clean-up, for pre-concentration and determination of carbamazepine in biological samples. The synthesized adsorbent also showed high selectivity to carbamazepine compared to other drugs with similar structure. Important factors affecting the extraction efficiency of the analyte in the in-tube SPME method, such as salt concentration, extraction and desorption times, flowrates of the sample solution, and eluent, were optimized. Under optimal conditions, the method showed good linearity for carbamazepine in the range of 0.05-500 μg L, 0.10-500 μg L, and 0.10-500 μg L in water, urine, and plasma samples, respectively, with coefficients of determination better than 0.996. The limits of detection were in the range of 0.01-0.05 μg L in different matrices. The intra- and inter-assay precisions (RSD%, n = 3) were in the range of 6.7-8.1 % and 7.1-9.5 %, respectively.
一种分子印迹聚吡咯纳米复合材料（MIP@CuO）被引入作为一种新的管内固相微萃取（IT-SPME）涂层。该方法与 HPLC-UV 相结合，成功地应用于生物样品中卡马西平（抗惊厥和双相情感障碍药物）的分析。首先，为了提高涂层的表面积和稳定性，采用化学方法在铜管内表面合成了氧化铜（CuO）纳米片。然后，通过简单的原位电沉积方法在 CuO 上沉积了分子印迹聚吡咯涂层（以卡马西平为模板）。结果表明，MIP@CuO 涂层具有长寿命、增强的萃取效率和良好的净化效果，可用于生物样品中卡马西平的预浓缩和测定。与具有相似结构的其他药物相比，合成的吸附剂对卡马西平也表现出较高的选择性。影响管内 SPME 方法中分析物萃取效率的重要因素，如盐浓度、萃取和洗脱时间、样品溶液流速和洗脱液等，进行了优化。在最佳条件下，该方法在水、尿和血浆样品中对卡马西平的线性范围分别为 0.05-500 μg L、0.10-500 μg L 和 0.10-500 μg L，相关系数均大于 0.996。不同基质中的检测限在 0.01-0.05 μg L 范围内。内标和间标精密度（RSD%，n = 3）分别为 6.7-8.1%和 7.1-9.5%。
