School of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225002, China.
Analyst. 2012 May 21;137(10):2400-5. doi: 10.1039/c2an35300h. Epub 2012 Apr 10.
In this study, an automated sequential injection lab-on-valve (SI-LOV) system was designed for the on-line matrix removal and preconcentration of quercetin. Octadecyl functionalized magnetic silica nanoparticles were prepared and packed into the microcolumn of the LOV as adsorbents. After being adsorbed through hydrophobic interaction, the analyte was eluted and subsequently introduced into the electrochemical flow cell by voltammetric quantification. The main parameters affecting the performance of solid-phase extraction, such as sample pH and flow rate, eluent solution and volume, accumulation potential and accumulation time were investigated in detail. Under the optimum experimental conditions, a linear calibration curve was obtained in the range of 1.0 × 10(-8) to 1 × 10(-5) mol L(-1) with R(2) = 0.9979. The limit of detection (LOD) and limit of quantitation (LOQ) were 1.3 × 10(-9) and 4.3 × 10(-9) mol L(-1), respectively. The relative standard deviation (RSD) for the determination of 1.0 × 10(-6) mol L(-1) quercetin was found to be 2.9% (n = 11) along with a sampling frequency of 40 h(-1). The applicability and reliability of the automated method described here had been applied to the determination of quercetin in human urine and red wine samples through recovery experiments, and the obtained results were in good agreement with those obtained by the HPLC method.
本研究设计了一种自动化顺序注射阀上实验室(SI-LOV)系统,用于槲皮素的在线基质去除和预浓缩。十八烷基功能化磁性硅胶纳米粒子被制备并填充到 LOV 的微柱中作为吸附剂。通过疏水相互作用吸附后,分析物被洗脱,随后通过伏安定量法引入电化学流动池。详细研究了影响固相萃取性能的主要参数,如样品 pH 值和流速、洗脱液和体积、积累电位和积累时间。在最佳实验条件下,在 1.0×10(-8)至 1.0×10(-5) mol L(-1)范围内得到了线性校准曲线,R(2)为 0.9979。检测限(LOD)和定量限(LOQ)分别为 1.3×10(-9)和 4.3×10(-9) mol L(-1)。对于 1.0×10(-6) mol L(-1)槲皮素的测定,相对标准偏差(RSD)为 2.9%(n = 11),采样频率为 40 h(-1)。通过回收率实验,将所描述的自动化方法的适用性和可靠性应用于人尿和红酒样品中槲皮素的测定,所得结果与 HPLC 法一致。