Simultaneous determination of microcystin-LR and its glutathione conjugate in fish tissues by liquid chromatography-tandem mass spectrometry.
A sensitive and selective liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous quantitative determination of microcystin-LR (MC-LR) and its glutathione conjugate (MC-LR-GSH) in fish tissues. The analytes were extracted from fish liver and kidney using 0.01M EDTA-Na(2)-5% acetic acid, followed by a solid-phase extraction (SPE) on Oasis HLB and silica cartridges. High-performance liquid chromatography (HPLC) with electrospray ionization mass spectrometry, operating in selected reaction monitoring (SRM) mode, was used to quantify MC-LR and its glutathione conjugate in fish liver and kidney. Recoveries of analytes were assessed at three concentrations (0.2, 1.0, and 5microg g(-1) dry weight [DW]) and ranged from 91 to 103% for MC-LR, and from 65.0 to 75.7% for MC-LR-GSH. The assay was linear within the range from 0.02 to 5.0microg g(-1) DW, with a limit of quantification (LOQ) of 0.02microg g(-1) DW. The limit of detection (LOD) of the method was 0.007microg g(-1) DW in both fish liver and kidney. The overall precision was determined on three different days. The values for within- and between-day precision in liver and kidney were within 15%. This method was applied to the identification and quantification of MC-LR and its glutathione conjugate in liver and kidney of fish with acute exposure of MC-LR.
Dai
Ming
M
Donghu Experimental Station of Lake Ecosystems, State Key Laboratory of Freshwater Ecology and Biotechnology of China, Institute of Hydrobiology, Chinese Academy of Sciences, Donghu South Road 7, Wuhan 430072, PR China.
Xie
Ping
P
Liang
Gaodao
G
Chen
Jun
J
Lei
Hehua
H
D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005399:Fishes; D005978:Glutathione / Q000032:analysis* / Q000737:chemistry; D007668:Kidney / Q000737:chemistry; D008099:Liver / Q000737:chemistry; D008387:Marine Toxins; D052998:Microcystins / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods*
D008387:Marine Toxins; D052998:Microcystins; C057862:cyanoginosin LR; D005978:Glutathione