Qronfla Murad M, Jamoussi Bassem, Chakroun Radhouane, Al-Mur Bandar A, Halawani Riyadh F, Aloufi Fahed A
Department of Environment, Faculty of Environmental Sciences, King Abdulaziz University, Jeddah 21589, Saudi Arabia.
Polymers (Basel). 2023 Aug 2;15(15):3279. doi: 10.3390/polym15153279.
Styrene, a chemical widely used in various industries, undergoes metabolic breakdown in the human body, resulting in the production of phenylglyoxylic acid (PGA). A novel molecularly imprinted polymer (MIP) was synthesised for selective extraction and enrichment of PGA in urine samples prior to high-performance liquid chromatography. The MIP employed in this research was a 4-vinylpyridine molecularly imprinted polymer (4-VPMIP) prepared via mass polymerisation using a noncovalent method. The structural and morphological characteristics of the molecularly imprinted polymers (MIPs) and non-imprinted polymers (NIPs) were evaluated using Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). The efficiency of the molecularly imprinted solid-phase extraction (MISPE) process was optimised by investigating critical variables such as sample pH, sorbent mass, sample flow rate, and volume of the elution solvent. A central composite design (CCD) within the response surface methodology was utilised to develop separate models for the adsorption and desorption steps. Analysis of variance (ANOVA) confirmed the excellent fit of the experimental data to the proposed response models. Under the optimised conditions, the molecularly imprinted polymers exhibited a higher degree of selectivity and affinity for PGA, with a relative selectivity coefficient (α) of 2.79 against hippuric acid. The limits of detection (LOD) and quantification (LOQ) for PGA were determined to be 0.5 mg/L and 1.6 mg/L, respectively. The recoveries of PGA ranged from 97.32% to 99.06%, with a relative standard deviation (RSD) lower than 4.6%. Furthermore, MIP(4VP)SPE demonstrated the potential for recycling up to three times without significant loss in analyte recovery.
苯乙烯是一种广泛应用于各种行业的化学品，在人体内会发生代谢分解，产生苯甲酰甲酸（PGA）。合成了一种新型分子印迹聚合物（MIP），用于在高效液相色谱分析之前选择性萃取和富集尿液样本中的PGA。本研究中使用的MIP是通过非共价法本体聚合法制备的4-乙烯基吡啶分子印迹聚合物（4-VPMIP）。使用傅里叶变换红外光谱（FT-IR）和扫描电子显微镜（SEM）对分子印迹聚合物（MIP）和非印迹聚合物（NIP）的结构和形态特征进行了评估。通过研究样品pH值、吸附剂质量、样品流速和洗脱溶剂体积等关键变量，优化了分子印迹固相萃取（MISPE）过程的效率。利用响应面法中的中心复合设计（CCD）分别建立了吸附和解吸步骤的模型。方差分析（ANOVA）证实了实验数据与所提出的响应模型具有良好的拟合度。在优化条件下，分子印迹聚合物对PGA表现出更高的选择性和亲和力，相对于马尿酸的相对选择性系数（α）为2.79。PGA的检测限（LOD）和定量限（LOQ）分别确定为0.5 mg/L和1.6 mg/L。PGA的回收率在97.32%至99.06%之间，相对标准偏差（RSD）低于4.6%。此外，MIP(4VP)SPE显示出可循环使用多达三次而分析物回收率无显著损失的潜力。
