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. 2024;13(1):A0161.
doi: 10.5702/massspectrometry.A0161. Epub 2024 Dec 18.

Simple and Rapid HPLC-ICP-MS Method for the Simultaneous Determination of Cr(III) and Cr(VI) by Combining a 2,6-Pyridinedicarboxylic Acid Pre-Complexation Treatment

Akane Ito  1   2 , Kazuto Isamoto  2 , Yuhei Morishita  2 , Masaharu Tanimizu  2
Affiliations

Simple and Rapid HPLC-ICP-MS Method for the Simultaneous Determination of Cr(III) and Cr(VI) by Combining a 2,6-Pyridinedicarboxylic Acid Pre-Complexation Treatment

Akane Ito et al. Mass Spectrom (Tokyo). 2024.

Abstract

A simple and rapid analytical method was developed for the simultaneous determination of two chromium species, Cr(III) and Cr(VI), in the environmental waters by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). This study incorporated a chelating pretreatment with 2,6-pyridinedicarboxylic acid (PDCA) to convert Cr(III) species into a stable Cr(III)-PDCA anion complex, which was then separated from Cr(VI) oxyanion using an anion exchange column. Building on the fundamental analytical approach proposed by Shigeta et al. (doi: 10.2116/analsci.18P012), the mobile phase was optimized to ensure stability for ICP-MS detection, avoiding nonvolatile salts. Chromium species and chloride ions were effectively separated within 6 minutes at a flow rate of 0.6 mL min-1 with the optimized mobile phase, which consisted of 50 mmol L-1 ammonium acetate (pH 6.80) and 2 mmol L-1 PDCA. The detection limits were 0.18 μg L-1 and 0.09 μg L-1 for Cr(III) and Cr(VI), respectively, at m/z 52 under He collision mode.

Keywords: HPLC-ICP-MS; PDCA; chromium; speciation; volatile salt mobile phase.

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Figures

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Fig. 1. Chromatograms of 100 μg L−1 Cr(III)-PDCA and Cr(VI) for m/z 52 at pH 6.22 (light gray), 6.41 (gray), 6.71 (dark gray), and 7.03 (black) under the flow rate of 0.3 mL min−1. PDCA, 2,6-pyridinedicarboxylic acid.
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Fig. 2. Signals (peak area) of Cr(III) (open triangle) and Cr(VI) (mesh triangle) and peak area ratio of Cr(III)/Cr(VI) (closed circle) at pH 6.22, 6.41, 6.71, and 7.03.
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Fig. 3. Chromatograms of 10 μg L−1 Cr(III)-PDCA and Cr(VI) for m/z 52, using a pH 6.80 mobile phase and a flow rate of 0.5 mL min−1 (light gray), 0.6 mL min−1 (gray), and 0.7 mL min−1 (black) with the chromatogram of 210 mg L−1 Cl for m/z 35 at a flow rate of 0.6 mL min−1 (gray). PDCA, 2,6-pyridinedicarboxylic acid.
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Fig. 4. Calibration curves for Cr(III) (closed circle) and Cr(VI) (open circle) under optimized HPLC and ICP-MS conditions.
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