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. 2022 Dec 27;94(51):18042-18049.
doi: 10.1021/acs.analchem.2c04458. Epub 2022 Dec 15.

High-Throughput Determination of Ultratrace Actinides in Urine by In-Line Extraction Chromatography Combined with Quadrupole Inductively Coupled Plasma Mass Spectrometry (EC-ICP-MS)

Affiliations

High-Throughput Determination of Ultratrace Actinides in Urine by In-Line Extraction Chromatography Combined with Quadrupole Inductively Coupled Plasma Mass Spectrometry (EC-ICP-MS)

Yongzhong Liu et al. Anal Chem. .

Abstract

Determining actinides in urine is vital for occupational exposure monitoring and radiological emergency response because of the toxicity and radiological dose effects of actinides on human health. Traditional radiochemistry analytical methods used to determine actinide concentrations in urine are time-consuming (sample analysis takes several days) and are hindered by a variety of technical and instrumentation-related obstacles. A high-throughput, fully automated, precise, and accurate in-line method was developed for determining five actinides (241Am, 239Pu, 237Np, 232Th, and 238U) at ng/L levels in urine using extraction chromatography combined with quadrupole inductively coupled plasma mass spectrometry (EC-ICP-MS). In this method, the five actinides were successfully separated with the required sensitivity, peak shape, and resolution using a simplified single Eichrom TRU column with a Dionex ICS-5000 system. The separated actinides were subsequently injected into an in-line PerkinElmer (PE) NexION 300D ICP-MS for quantitative determination. The sample-to-sample run time was 23 min for automatic chemical separation and quantification using only 0.5 mL of urine. The limits of detection (LOD) obtained using this method were 0.015, 0.022, 0.039, 4.5, and 2.4 ng/L for 241Am, 239Pu, 237Np, 232Th, and 238U, respectively. The method routinely had a chemical yield of >84% as well as a linearity (R2) coefficient of ≥0.999 for the calibrators. The method proved to be rapid, reliable, and effective for actinide quantification in urine and therefore is appropriate for radiological emergency response incidents.

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Figures

Figure 1.
Figure 1.
Flow schematic of actinides analysis by EC-ICP-MS. EC-ICP-MS: Extraction Chromatography Quadrupole Inductively Coupled Plasma Mass Spectrometry; Gilson: Peristaltic pump; TC: Thermal compartment; AS-AP: Autosampler; SP: Single gradient pump.
Figure 2.
Figure 2.
Chromatogram of 241Am, 239Pu, 237Np, 232Th, and 238U spiked in base urine separated using a Dionex ICS-5000 with a HPLC column containing TRU resin.

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