PMID- 24929550 OWN - NLM STAT- MEDLINE DCOM- 20150212 LR - 20201209 IS - 1873-376X (Electronic) IS - 1570-0232 (Linking) VI - 963 DP - 2014 Jul 15 TI - Simultaneous quantitative determination of microcystin-LR and its glutathione metabolites in rat liver by liquid chromatography-tandem mass spectrometry. PG - 54-61 LID - S1570-0232(14)00361-4 [pii] LID - 10.1016/j.jchromb.2014.05.046 [doi] AB - The roles of glutathione (GSH) and cysteine (Cys) in the detoxification of Microcystin-LR (MC-LR) have recently become a popular area of research. However, lacking analysis methods for MC-LR-GSH and MC-LR-Cys (two main GSH pathway metabolites) in mammals, elucidation of the detoxification mechanism and metabolic pathway of MC-LR in mammals is difficult. In this study, a novel method for the simultaneous quantitative analysis of MC-LR, MC-LR-GSH and MC-LR-Cys in rat liver was developed and validated. The analytes were simultaneously extracted from rat liver using 3M sodium chloride solution containing 0.01M EDTA-Na2-5% acetic acid, followed by solid-phase extraction (SPE) on Oasis HLB and silica cartridges and determination by liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS/MS). Under the optimized pretreatment conditions and instrument parameters, good recoveries of MC-LR, MC-LR-GSH and MC-LR-Cys were obtained at three concentrations (0.2, 1.0 and 2.5 mug g(-1) dry weight (DW)) with values ranging from 97.7 +/- 4.2 to 98.7 +/- 5.1%, 70.1 +/- 4.8 to 71.1 +/- 4.1% and 79.8 +/- 3.5 to 81.4 +/- 4.0%, respectively. The relative standard deviations (RSDs) of these compounds at 0.2, 1.0 and 2.5 mug g(-1) DW were between 4.3% and 6.9%. The limits of detection (LODs) were 0.005, 0.007 and 0.006 mug g(-1) DW and the limits of quantification (LOQs) were 0.017, 0.023 and 0.020 mug g(-1) DW for MC-LR, MC-LR-GSH and MC-LR-Cys, respectively. Furthermore, this method was successfully applied to both time- and dosage-effect studies of MC-LR, MC-LR-GSH and MC-LR-Cys in vivo. CI - Copyright (c) 2014 Elsevier B.V. All rights reserved. FAU - Guo, Xiaochun AU - Guo X AD - College of Fisheries, Huazhong Agricultural University, Wuhan, Hubei 430070, China. Electronic address: guoxiaochun419@163.com. FAU - Xie, Ping AU - Xie P AD - 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, China. Electronic address: xieping@ihb.ac.cn. FAU - Chen, Jun AU - Chen J AD - 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, China. Electronic address: chenjun@ihb.ac.cn. FAU - Tuo, Xun AU - Tuo X AD - 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, China. FAU - Deng, Xuwei AU - Deng X AD - 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, China. FAU - Li, Shangchun AU - Li S AD - 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, China. FAU - Yu, Dezhao AU - Yu D AD - 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, China. FAU - Zeng, Cheng AU - Zeng C AD - College of Fisheries, Huazhong Agricultural University, Wuhan, Hubei 430070, China. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PT - Validation Study DEP - 20140602 PL - Netherlands TA - J Chromatogr B Analyt Technol Biomed Life Sci JT - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JID - 101139554 RN - 0 (Marine Toxins) RN - 0 (Microcystins) RN - EQ8332842Y (cyanoginosin LR) RN - GAN16C9B8O (Glutathione) SB - IM MH - Animals MH - Chromatography, Liquid/methods MH - Glutathione/*analysis/*metabolism MH - Limit of Detection MH - Liver/*metabolism MH - Male MH - Marine Toxins MH - Microcystins/*analysis/*metabolism MH - Rats MH - Rats, Sprague-Dawley MH - Solid Phase Extraction/methods MH - Spectrometry, Mass, Electrospray Ionization/methods MH - Tandem Mass Spectrometry/methods OTO - NOTNLM OT - LC-ESI-MS/MS OT - Microcystin-LR OT - Microcystin-LR-Cys OT - Microcystin-LR-GSH OT - Quantitative determination OT - Rat liver EDAT- 2014/06/16 06:00 MHDA- 2015/02/13 06:00 CRDT- 2014/06/16 06:00 PHST- 2014/02/07 00:00 [received] PHST- 2014/05/18 00:00 [revised] PHST- 2014/05/23 00:00 [accepted] PHST- 2014/06/16 06:00 [entrez] PHST- 2014/06/16 06:00 [pubmed] PHST- 2015/02/13 06:00 [medline] AID - S1570-0232(14)00361-4 [pii] AID - 10.1016/j.jchromb.2014.05.046 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jul 15;963:54-61. doi: 10.1016/j.jchromb.2014.05.046. Epub 2014 Jun 2.