Switchable metal extractant integrated miniaturized 3D-printed device: A semi-online multi-metal separation system for matrix-free ICP-MS analysis.

Background: This study tackles the critical challenges in metal analysis by presenting an innovative miniaturized metal extraction device prototype. This device features a functional nanocomposite (FNC) enhanced 3D-printed polylactic acid (PLA) metal extractant (FNC@3D PLA). The research is motivated by the constraints of traditional solid-phase extraction (SPE) methods, specifically their limitations in handling competitive metal ion environments and matrix interference during inductively coupled plasma mass spectrometry (ICP-MS) analysis. The designed prototype aims to overcome these challenges and enhance the extraction efficiency of diverse metals.

Results: The FNC, designed to incorporate various functional groups critical for metal ion extraction efficiency, was meticulously engineered through the reaction of acid-treated and delaminated graphitic carbon nitride nanosheets (Thiol-gCN NSs) with 3-mercaptopropyl trimethoxysilane (MPTMS). The competitive metal ion extraction efficiency of FNC@3D PLA was demonstrated, showcasing notable limit of detection values of 3.2 ± 0.7 ng mL and 8.57 ± 3.05 ng mL for Cu and Ag, respectively. Furthermore, the miniaturized 3D-printed metal-preconcentration setup incorporating FNC@3D PLA exhibited favorable intraday relative standard deviation (RSD) percentage (%) values ranging from 1.23 to 8.6 for both Cu and Ag. Interday RSD % between 1.41 and 8.14 were observed under spiked real urine sample conditions. The sustainability and robustness of the proposed approach were underscored by substantial recovery % values exhibited by FNC@3D PLA, even after eight consecutive regeneration processes.

Significance: This study significantly contributes to the advancement of analytical methodologies by providing a reliable and efficient platform for metal extraction and preconcentration in practical metal analysis applications. Developed FNC@3D PLA system demonstrates its potential to address the challenges associated with SPE in metal analysis, especially in complex sample matrices. We believe implications of this research can be extended to various fields, from environmental monitoring to clinical diagnostics, where accurate and reliable metal analysis is paramount.