Key Laboratory of Analysis and Detection Technology for Food Safety, Ministry of Education, Fuzhou University, Fuzhou, P. R. China.
Electrophoresis. 2013 Jul;34(14):2049-57. doi: 10.1002/elps.201200703. Epub 2013 Jun 20.
A simple analysis of chlorophenols (2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, and pentachlorophenol) and phenol was accomplished by coupling a pressurized CEC with amperometric detection (AD). Efficient and reproducible separation of these compounds was achieved within 9 min on a capillary monolithic stationary phase bonded with octadecyl ligands and sulfonate groups, where the selectivity and the retention of analytes can be functionally controlled by optimizing experimental variables, including organic modifier content, mobile phase pH, ionic strength, working electrode potential, separation voltage, and supplementary pressure. A mixed-mode retention mechanism consisting of reverse-phase chromatographic partition, electrostatic repulsion, and electrophoresis is considered to play roles in the separation. The use of ACN-based media seems effectual in preventing the unfavorable irreversible adsorption on both wall and electrode, and offer higher sensitivity and less electrode fouling in AD of phenols. The LODs were in the range from 0.02 to 0.2 μg/mL with a wide linear dynamic range of 5000-fold, while the peak area precision ranged from 3.2 to 7.5%. The feasibility of using this method in real analysis was evaluated by recovery estimates and comparative experiment on spiked tap water samples. Good recoveries of 80-110% were achieved. Additionally, a paired t-test was used to correlate the two methods.
采用加压毛细管电泳与安培检测（AD）联用的方法，对氯酚（2-氯酚、2,4-二氯酚、2,4,6-三氯酚和五氯酚）和苯酚进行了简单分析。在十八烷基键合和磺酸基团键合的毛细管整体固定相上，这些化合物在 9 分钟内得到了高效且重现的分离，通过优化实验变量（包括有机改性剂含量、流动相 pH 值、离子强度、工作电极电位、分离电压和辅助压力），可以实现对分析物的选择性和保留的功能控制。认为分离过程中存在一种由反相色谱分配、静电排斥和电泳组成的混合模式保留机制。使用基于 ACN 的介质似乎可以有效地防止在管壁和电极上发生不利的不可逆吸附，并在 AD 中提供更高的灵敏度和更少的电极污染。LOD 范围为 0.02-0.2μg/mL，线性动态范围为 5000 倍，峰面积精密度范围为 3.2-7.5%。通过对加标自来水样品进行回收估计和比较实验，评估了该方法在实际分析中的可行性。回收率为 80-110%。此外，还使用配对 t 检验对两种方法进行了相关性分析。
