Abstract

A fully automated on-line sample pretreatment system combining microwave digestion with sample preconcentration/matrix separation for the determination of trace metals (Fe, Ni, Cu, Zn, and Pb) in blood and serum samples by inductively coupled plasma mass spectrometry (ICPMS) was designed and evaluated. The samples were mixed with an appropriate reagent and digested in a flow-through, focused microwave-heated oven. After digestion, the sample solution was transferred on-line to a column packed with iminodiacetate-based resin for separation of matrix elements like Na, K, Ca, Mg, Cl, P, and S that might interfere with the measurement by ICPMS. The analytes chelated on the resin were subsequently eluted and led to ICPMS for multielement determination. The whole sample pretreatment process was automatically controlled by a self-designed expert system. The analytical reliability of data from this on-line system was confirmed to be good with the analysis of SRM samples (Seronorm Whole Blood and NIST SRM 1598 Bovine Serum), and the limits of detection (3 sigma) for Fe, Ni, Cu, Zn, and Pb were 68, 0.34, 3.5, 13.4, and 0.22 microgram/L, respectively. With this fully automated on-line system, the determination of analytes in biological fluid samples down to micrograms-per-liter levels has been proven to be feasible, and the sample throughput can achieve up to 6 samples/h.

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