title: 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.
abstract: 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 (50-2000ng/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.
authors.affiliation: CAS Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Zhongshan Road 457, Dalian, China.
authors.forename: Yuanhong
authors.initials: Y
authors.lastname: Shan
authors.forename: Xianzhe
authors.initials: X
authors.lastname: Shi
authors.forename: Abo
authors.initials: A
authors.lastname: Dou
authors.forename: Cunjie
authors.initials: C
authors.lastname: Zou
authors.forename: Hongbing
authors.initials: H
authors.lastname: He
authors.forename: Qin
authors.initials: Q
authors.lastname: Yang
authors.forename: Sumin
authors.initials: S
authors.lastname: Zhao
authors.forename: Xin
authors.initials: X
authors.lastname: Lu
authors.forename: Guowang
authors.initials: G
authors.lastname: Xu
mesh_terms: D001331:Automation / Q000379:methods*; D053801:Capillary Electrochromatography; D005618:Fresh Water; D057166:High-Throughput Screening Assays / Q000295:instrumentation* / Q000379:methods*; D016014:Linear Models; D052998:Microcystins / Q000032:analysis*; D010456:Peptides, Cyclic / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052617:Solid Phase Microextraction; D053719:Tandem Mass Spectrometry; D014867:Water; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D052998:Microcystins; D010456:Peptides, Cyclic; D014874:Water Pollutants, Chemical; D014867:Water; C063998:nodularin