Published: Journal of Chromatographic
Science, ISSN 0021-9665 Volume
44, Number 6, July 2006, pp.359-365
Determination of Microcystins in Water Using Integrated
Solid-Phase Microextraction with Microbore High-Performance Liquid
ChromatographyElectrospray Quadruple Time-of-Flight Mass Spectrometry
Yuan-Yuan Zhao, Steve Hrudey, and Xing-Fang Li
Environmental Health Sciences, Department of Public Health Sciences,
Faculty of Medicine and Dentistry, University of Alberta, Canada
T6G 2G3
The development
of a technique combining solid-phase microextraction (SPME) with
microbore high-performance liquid chromatography (micro-HPLC)tandem
quadrupole time-of-flight (QTOF) mass spectrometry (MS) for determination
of dissolved microcystins in water is reported. Several important
parameters affecting the efficiency of SPME extraction of microcystins
are investigated. A microbore C18 column HPLC coupled with tandem
QTOF-MS with information-dependent acquisition (IDA) is developed
to effectively analyze microcystins in microliter volumes of SPME
extracts. The micro-HPLCQTOF-MS with IDA technique provides comprehensive
information, including a survey chromatogram (total ion chromatogram),
full scan mass spectrum, and product ion scan mass spectra at
different collision energies for individual analytes, which allows
for both identification and quantitation in the same run. Linear
calibration curves of microcystin standard [microcystin (MC)-arginine
(R)R] 1100 µg/L and of microcystin standard [MC-leucine (L)R]
1250 µg/L are obtained with a correlation coefficient of 0.996.
The combination of SPME with HPLCQTOF-MS and IDA offers limits
of detection of 0.6 pg for MC-RR and 1.6 pg for MC-LR. Analysis
of spiked lake-water samples shows a recovery of > 86% for MC-RR
and > 70% for MC-LR. This technique requires small sample volumes,
minimizes the use of organic solvents, and provides sensitive
and information-rich analysis of unknown samples. .
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