Yokota Yuki, Gemmei-Ide Makoto, Inoue Yoshinori, Kagaya Shigehiro
Faculty of Engineering, University of Toyama, Toyama, 930-8555, Japan.
Anal Sci. 2023 Apr;39(4):589-600. doi: 10.1007/s44211-023-00277-w. Epub 2023 Feb 7.
An automated system for the rapid separation and preconcentration of trace elements was developed. Carboxymethylated polyethyleneimine 600 (CM-PEI600), which is a partially carboxymethylated polyethyleneimine with a molecular weight of 600 Da, was used as a chelating resin to quantitatively recover trace elements under high-flow-rate conditions. For accurately and precisely determining trace elements, even with a rough control of the sample and eluent flow volumes, an internal standardization technique was employed for the solid-phase extraction and separation. A recovery test of the deionized water-based sample solution was conducted using this system, and good results, with a recovery of 92% or higher, were obtained for 11 elements (Cd, Co, Cu, Fe, Mn, Mo, Ni, Pb, Ti, V, and Zn). Eight elements present in certified groundwater and wastewater reference materials (ES-L-1 and EU-L) were separated and preconcentrated using this system. Almost all the determined values were within their tolerance intervals, and no significant differences were observed between the determined and certified values, demonstrating the validity of this method. The time required for the separation and preconcentration using approximately 100 mL of the sample solution was approximately 6.5 min, and theoretically, the system could be used to preconcentrate 17 samples in an hour because extraction and elution could be conducted simultaneously using two cartridges packed with the chelating resin. Using this system equipped with cartridges packed with CM-PEI600 resin, solid-phase extraction and the separation of multiple elements were performed simultaneously, automatically, and rapidly, enabling the accurate and precise determination of trace elements in environmental water and inorganic salts even by rapidly flowing the sample solutions using peristaltic pumps. Compared to NOBIAS Chelate PA-1, a commercially available chelating resin, the CM-PEI600 resin can recover trace elements even under an extremely high flow rate of approximately 50 mL min.
开发了一种用于快速分离和预富集痕量元素的自动化系统。羧甲基化聚乙烯亚胺600(CM-PEI600),即一种分子量为600 Da的部分羧甲基化聚乙烯亚胺,被用作螯合树脂,以在高流速条件下定量回收痕量元素。为了准确精确地测定痕量元素,即使对样品和洗脱液的流量进行粗略控制,在固相萃取和分离中采用了内标技术。使用该系统对去离子水基样品溶液进行了回收率测试,对于11种元素(镉、钴、铜、铁、锰、钼、镍、铅、钛、钒和锌)获得了良好的结果,回收率达到92%或更高。使用该系统对认证地下水和废水标准物质(ES-L-1和EU-L)中存在的8种元素进行了分离和预富集。几乎所有测定值都在其允许区间内,测定值与认证值之间未观察到显著差异,证明了该方法的有效性。使用约100 mL样品溶液进行分离和预富集所需的时间约为6.5分钟,理论上,该系统每小时可用于预富集17个样品,因为萃取和洗脱可使用两个装有螯合树脂的柱同时进行。使用配备装有CM-PEI600树脂柱的该系统,可同时、自动且快速地进行多种元素的固相萃取和分离,即使使用蠕动泵快速流动样品溶液,也能准确精确地测定环境水和无机盐中的痕量元素。与市售螯合树脂NOBIAS Chelate PA-1相比,CM-PEI600树脂即使在约50 mL/min的极高流速下也能回收痕量元素。