Abstract

A molecularly imprinted polymer (MIP) of carbamazepine (CBZ) was synthesized so as to facilitate the selective extraction of CBZ from aqueous and bio-samples by using a non-covalent imprinting approach. Synthesized materials were characterized with Fourier-transform infrared spectroscopy and scanning electron microscopy studies. The imprinted polymer was evaluated and applied as a sorbent for solid-phase extraction (SPE) coupled with HPLC-UV to detect CBZ and its metabolite oxcarbazepine (OXC). The optimal conditions for molecularly imprinted SPE (MISPE) consist of the cartridge conditioning using methanol followed by triply distilled water, loading the aqueous sample and elution by methanol-acetic acid (9 : 1, v/v). The selectivity and sensitivity for pre-concentration and separation of the target analytes were studied in details, in order to build a simple and sensitive method which can act as a potential analytical strategy to monitor CBZ and OXC in the environmental and biological samples. The developed method exhibited a wide linear range (1–500 μg/L), good linearity (R² > 0.990), and relative standard deviation <3%. The molecular recognition properties of the MIP gave rise to good recoveries for CBZ (87–98%) and OXC (72–78%) when spiked aqueous and bio-samples were percolated through the MISPE procedure. The limit of detection for CBZ and OXC were 0.488 and 0.515 μg/L, respectively. Moreover, each MISPE cartridge, when investigated for reusability test, displayed excellent recoveries for CBZ (98–94%) with enhanced reusability (10 cycles).

中文翻译：

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分子印迹聚合物对水和生物样品中卡马西平和奥卡西平的有效识别和测定

摘要

合成了卡马西平（CBZ）的分子印迹聚合物（MIP），以利于通过使用非共价印迹方法从水性和生物样品中选择性提取CBZ。通过傅立叶变换红外光谱和扫描电子显微镜研究对合成材料进行表征。对印迹聚合物进行评估，并将其用作固相萃取（SPE）的吸附剂，并与HPLC-UV联用，以检测CBZ及其代谢产物奥卡西平（OXC）。分子印迹SPE（MISPE）包括使用甲醇和随后的三倍蒸馏水进行柱调节，加载水性样品并通过甲醇-乙酸（9：1，v / v）洗脱的步骤。为了建立一种简单而灵敏的方法，该方法可作为监测环境和生物样品中CBZ和OXC的潜在分析策略，详细研究了目标分析物的预浓缩和分离的选择性和灵敏度。所开发的方法具有较宽的线性范围（1-500μg/ L），良好的线性（R ²> 0.990），相对标准偏差<3％。当通过MISPE程序对加标的水样和生物样品进行渗滤时，MIP的分子识别特性可提高CBZ（87-98％）和OXC（72-78％）的回收率。CBZ和OXC的检出限分别为0.488和0.515μg/ L。此外，每个MISPE弹药筒在进行可重复使用性测试时，都显示出CBZ的优异回收率（98-94％），并具有增强的可重复使用性（10个循环）。