Shanghai Key Laboratory of Functional Materials Chemistry, School of Chemistry and Molecular Engineering, East China University of Science and Technology, Shanghai 200237, China.
School of Biotechnology, East China University of Science and Technology, Shanghai 200237, China.
J Chromatogr A. 2021 Jul 5;1648:462192. doi: 10.1016/j.chroma.2021.462192. Epub 2021 Apr 27.
Determination of folic acid and riboflavin in biological samples is difficult due to their high polarity, low concentration, chemical instability, and complex matrix. In this study, the polypyrrole-coated magnetic nanocomposite (FeO@PPy) was synthesized innovatively with the assistance of hexadecyltrimethylammonium bromide. To evaluate the adsorption mechanism and the feasibility of synthesized FeO@PPy as an adsorbent, the adsorption capacities, kinetics and thermodynamics of folic acid and riboflavin were investigated systemically. Furthermore, in light of the chemical instability of folic acid and riboflavin a method for rapid extraction and detection of them from human urine within 10 min was developed successfully by combining magnetic solid phase extraction with ultra-performance liquid chromatography (MSPE/UPLC). The adsorption parameters including sorbent amount, pH value, extraction time, desorption solvent and desorption time were studied. Under optimum conditions, the performance of the established determination method was validated with the linearly dependent coefficients (>0.9995), the limits of detection (0.02-0.05 µg/mL), the limits of quantification (0.07-0.18 µg/mL), and the recoveries (92.2-105.1%, with relative standard deviation < 3.3%). The rapid extraction and detection of folic acid and riboflavin from real urine samples were achieved subsequently. The present study suggests that the developed method exhibits a promising application in the analysis of free folic acid and riboflavin in human urine samples, which can provide a reference for the clinical drug monitoring and treatment.
由于其高极性、低浓度、化学不稳定性和复杂基质,生物样品中叶酸和核黄素的测定较为困难。本研究创新性地利用十六烷基三甲基溴化铵辅助合成了聚吡咯包覆的磁性纳米复合材料(FeO@PPy)。为了评估吸附机制和合成的 FeO@PPy 作为吸附剂的可行性,系统研究了叶酸和核黄素的吸附容量、动力学和热力学。此外,鉴于叶酸和核黄素的化学不稳定性,成功地开发了一种结合磁固相萃取和超高效液相色谱(MSPE/UPLC)从人尿中快速提取和检测它们的方法。研究了吸附参数,包括吸附剂用量、pH 值、提取时间、解吸溶剂和解吸时间。在最佳条件下,通过线性相关系数(>0.9995)、检测限(0.02-0.05 µg/mL)、定量限(0.07-0.18 µg/mL)和回收率(92.2-105.1%,相对标准偏差 < 3.3%)验证了所建立的测定方法的性能。随后,从真实尿液样品中快速提取和检测叶酸和核黄素。本研究表明,所开发的方法在分析人尿液样品中的游离叶酸和核黄素方面具有广阔的应用前景,可为临床药物监测和治疗提供参考。