Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, E-23071 Jaén, Spain.
Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, E-23071 Jaén, Spain.
Talanta. 2018 May 15;182:267-272. doi: 10.1016/j.talanta.2018.01.091. Epub 2018 Feb 2.
In this work, the implementation of Bead Injection with multicommutation-based flow systems is reported. A surface renewable chemiluminescence (CL) flow sensor is presented based on the use of CL reaction of luminol with HO. Dowex 1 × 8 beads with immobilized luminol onto them were injected in the flow system by means of a six-port rotary valve and were accommodated into a 1 mm optical glass flow cell placed just in front of the rectangular photosensor window with the same size than the cell wall. Automatic computer-controlled manipulation of both reagents and sample solutions was undertaken using a multicommutated flow system which comprises five three-way solenoid valves, a home-made electronic interface and a Java-written software. Once the chemiluminescence signal was registered, sensing beads were automatically discarded out with a six-port rotary valve without needing to reverse or stop the flow. As a proof of concept and example, the enhancement of the chemiluminescence signal produced by Co(II) on the luminol-HO reaction in alkaline medium was used for illustrating this implementation determining vitamin B in pharmaceutical preparations (after mineralization for releasing Co(II)). The analytical performance of the approach was satisfactory, showing a linear dynamic range from 1.7 to 50 µg L, a detection limit of 0.5 µg L, RSD (%) of 5.3%, with a sampling frequency of 11 h. The proposed approach was applied to different samples and the results were consistent with those obtained with a reference method based on ICP-MS. Based on the same reaction (or re-configuring the system to accommodate it to reaction requirements) the approach can also be applied to the determination of other metal ions such as Cr(III) and Fe(II) and appropriately extended to molecules of bioanalytical interest based e.g. in CL immunoassays, given its versatility.
在这项工作中,报告了基于多切换的流动系统的胶珠注入的实现。提出了一种基于鲁米诺与 HO 反应的表面可再生化学发光(CL)流动传感器。将固定有鲁米诺的 Dowex 1 × 8 珠通过六通旋转阀注入流动系统,并容纳在一个 1mm 光学玻璃流动池中,该流动池正好位于与池壁大小相同的矩形光电传感器窗口前。使用多切换流动系统自动进行两种试剂和样品溶液的计算机控制操作,该系统包括五个三通电磁阀、自制电子接口和用 Java 编写的软件。一旦记录到化学发光信号,就通过六通旋转阀自动丢弃传感珠,而无需反向或停止流动。作为概念验证和示例,使用 Co(II)在碱性介质中对鲁米诺-HO 反应产生的化学发光信号增强来举例说明这种实施方式,用于测定药物制剂中的维生素 B(通过矿化释放 Co(II)后)。该方法的分析性能令人满意,显示出从 1.7 到 50µg/L 的线性动态范围、检测限为 0.5µg/L、RSD(%)为 5.3%,采样频率为 11h。该方法已应用于不同的样品,结果与基于 ICP-MS 的参考方法一致。基于相同的反应(或重新配置系统以适应反应要求),该方法还可用于测定其他金属离子,如 Cr(III)和 Fe(II),并根据其多功能性适当扩展到生物分析感兴趣的分子,例如在 CL 免疫分析中。