A fully automated system with on-line micro solid-phase extraction combined with capillary liquid chromatography–tandem mass spectrometry for high throughput analysis of microcystins and nodularin-R in tap water and lake water

• Published in: Journal of Chromatography A Vol. 1218; no. 13; pp. 1743 - 1748
• Main Authors: Shan, Yuanhong, Shi, Xianzhe, Dou, Abo, Zou, Cunjie, He, Hongbing, Yang, Qin, Zhao, Sumin, Lu, Xin, Xu, Guowang
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 01.04.2011; Elsevier
• Subjects: Analytical chemistry; Applied sciences; Automation - methods; Capillary Electrochromatography; Capillary liquid chromatography–mass spectrometry; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography; detection limit; Drinking water and swimming-pool water. Desalination; Exact sciences and technology; Fresh Water; Freshwater; guidelines; hepatotoxins; High-Throughput Screening Assays - instrumentation; High-Throughput Screening Assays - methods; Lakes; Linear Models; liquid chromatography; Liquids; Mass spectrometry; microcystin-LR; Microcystins; Microcystins - analysis; Monitoring; neoplasms; Nodularin-R; On-line micro solid-phase extraction; On-line systems; Other chromatographic methods; Peptides, Cyclic - analysis; Pollution; Reproducibility of Results; Sensitivity and Specificity; solid phase extraction; Solid Phase Microextraction; Tandem Mass Spectrometry; Tap water; Toxins; Water; Water Pollutants, Chemical - analysis; water quality; Water treatment and pollution; World Health Organization; Capillary liquid chromatography–mass spectrometry; On-line micro solid-phase extraction; Microcystins; Nodularin-R; Capillary column; High throughput screening; Tandem mass spectrometry; Chemical analysis; On line; Cyclic peptides; HPLC chromatography; Electrospray; Chemical enrichment; Sample preparation; Quantitative analysis; Trace analysis; Validation; Automation; Coupled method; Tap water; Solid phase microextraction; Toxin; Capillary liquid chromatography-mass spectrometry; Surface water; Water quality; Water pollution
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2011.01.069

Microcystins and nodularins are cyclic peptide hepatotoxins and tumour promoters from cyanobacteria. The present study describes the development, validation and practical application of a fully automated analytical method based on on-line micro solid-phase extraction–capillary liquid chromatography–tandem mass spectrometry for the simultaneous determination of seven microcystins and nodularin-R in tap water and lake water. Aliquots of just 100 μL of water samples are sufficient for the detection and quantification of all eight toxins. Selected reaction monitoring was used to obtain the highest sensitivity. Good linear calibrations were obtained for microcystins (50–2000 ng/L) and nodularin-R (25–1000 ng/L) in spiked tap water and lake water samples. Excellent interday and intraday repeatability were achieved for eight toxins with relative standard deviation less than 15.7% in three different concentrations. Acceptable recoveries were achieved in the three concentrations with both tap water matrix and lake water matrix and no significant matrix effect was found in tap water and lake water except for microcystin-RR. The limits of detection (signal to noise ratio = 3) of toxins were lower than 56.6 ng/L which is far below the 1 μg/L defined by the World Health Organization provisional guideline for microcystin-LR. Finally, this method was successfully applied to lake water samples from Tai lake and proved to be useful for water quality monitoring.