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Issue 13, 2017
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Improved solid-phase extraction protocol and sensitive quantification of six microcystins in water using an HPLC-orbitrap mass spectrometry system

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Abstract

A solid-phase extraction (SPE) protocol was developed and combined with HPLC-ESI-MS for the quantification of common cyanobacterial toxins, microcystins (MCs), in water. An HPLC binary gradient was established for the separation of MC-LR, MC-YR, MC-RR, MC-LA, MC-LW, and MC-LF, while quantification of MCs in MC-spiked HPLC-grade water, tap water, and lake water was achieved in selected ion monitoring (SIM) mode using a high-resolution Orbitrap Fusion Tribrid mass spectrometer. All MC ions were detected with high mass accuracy of ≤1.61 ppm using the orbitrap mass analyzer, and MCs were quantified using external calibration based on LC-SIM-MS peak areas of the monoisotopic MC ions. The LOQs of MC-LA, MC-LW, and MC-LF in water using LC-SIM-MS were ∼25 ng L−1 while LOQs of MC-RR, MC-LR and MC-YR in water were ∼10 ng L−1. After the purification and preconcentration of MCs by SPE, LOQs of MC-LA, MC-LW and MC-LF were improved to ∼1 ng L−1 and LOQs of MC-RR, MC-LR and MC-YR were improved to ∼600 pg L−1 in tap water and lake water. The percent recoveries of MCs after SPE and sample preconcentration were in the range from 97.1% to 100.9% with a relative standard deviation (RSD) of ≤5.0%, indicating that this is one of the most efficient and reproducible SPE procedures for recovery of MCs from aqueous solutions. Additionally, a parallel LC-tandem mass spectrometry (MS/MS) method was established for the structural identification of MCs. Overall, the MC purification and preconcentration method developed and LC-SIM-MS enable sensitive, selective, and reproducible identification and quantification of MCs in water using the MS and MS/MS capabilities of a high-mass accuracy orbitrap mass spectrometer.

Graphical abstract: Improved solid-phase extraction protocol and sensitive quantification of six microcystins in water using an HPLC-orbitrap mass spectrometry system

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Publication details

The article was received on 27 Dec 2016, accepted on 12 Feb 2017 and first published on 13 Feb 2017


Article type: Paper
DOI: 10.1039/C6AY03459D
Citation: Anal. Methods, 2017,9, 2021-2030
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    Improved solid-phase extraction protocol and sensitive quantification of six microcystins in water using an HPLC-orbitrap mass spectrometry system

    D. S. W. Palagama, R. E. West III and D. Isailovic, Anal. Methods, 2017, 9, 2021
    DOI: 10.1039/C6AY03459D

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