PMID- 30201162 OWN - NLM STAT- MEDLINE DCOM- 20181101 LR - 20181101 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1573 DP - 2018 Oct 26 TI - Development and applications of solid-phase extraction and liquid chromatography-mass spectrometry methods for quantification of microcystins in urine, plasma, and serum. PG - 66-77 LID - S0021-9673(18)31026-4 [pii] LID - 10.1016/j.chroma.2018.08.023 [doi] AB - The protocols for solid-phase extraction (SPE) of six microcystins (MCs; MC-LR, MC-RR, MC-LA, MC-LF, MC-LW, and MC-YR) from mouse urine, mouse plasma, and human serum are reported. The quantification of those MCs in biofluids was achieved using HPLC-orbitrap-MS in selected-ion monitoring (SIM) mode, and MCs in urine samples were also quantified by ultra-HPLC-triple quadrupole-tandem mass spectrometry (UHPLC-QqQ-MS/MS) in multiple reaction monitoring (MRM) mode. Under optimal conditions, the extraction recoveries of MCs from samples spiked at two different concentrations (1 mug/L and 10 mug/L) ranged from 90.4% to 104.3% with relative standard deviations (RSDs) /= 0.9950 for MC-LR, MC-RR and MC-YR, and R(2) >/= 0.9883 for MC-LA, MC-LF, and MC-LW. The limits of quantification (LOQs) in spiked urine samples were approximately 0.13 mug/L for MC-LR, MC-RR, and MC-YR, and approximately 0.50 mug/L for MC-LA, MC-LF, and MC-LW, while the LOQs in spiked plasma and serum were approximately 0.25 mug/L for MC-LR, MC-RR, and MC-YR, and approximately 1.00 mug/L for MC-LA, MC-LF, and MC-LW. The developed methods were applied in a proof-of-concept study to quantify urinary and blood concentrations of MC-LR after oral administration to mice. The urine of mice administered 50 mug of MC-LR per kg bodyweight contained on average 1.30 mug/L of MC-LR (n = 8), while mice administered 100 mug of MC-LR per kg bodyweight had average MC-LR concentration of 2.82 mug/L (n = 8). MC-LR was also quantified in the plasma of the same mice. The results showed that increased MC-LR dosage led to larger urinary and plasma MC-LR concentrations and the developed methods were effective for the quantification of MCs in mouse biofluids. CI - Copyright (c) 2018 Elsevier B.V. All rights reserved. FAU - Palagama, Dilrukshika S W AU - Palagama DSW AD - Department of Chemistry and Biochemistry, College of Natural Sciences and Mathematics, University of Toledo, Toledo, OH 43606, United States. FAU - Baliu-Rodriguez, David AU - Baliu-Rodriguez D AD - Department of Chemistry and Biochemistry, College of Natural Sciences and Mathematics, University of Toledo, Toledo, OH 43606, United States. FAU - Lad, Apurva AU - Lad A AD - Department of Medicine, Health Science Campus, University of Toledo Medical Center, Toledo, OH 43614, United States. FAU - Levison, Bruce S AU - Levison BS AD - Department of Physiology and Pharmacology, Health Science Campus, University of Toledo Medical Center, Toledo, OH 43614, United States. FAU - Kennedy, David J AU - Kennedy DJ AD - Department of Medicine, Health Science Campus, University of Toledo Medical Center, Toledo, OH 43614, United States. FAU - Haller, Steven T AU - Haller ST AD - Department of Medicine, Health Science Campus, University of Toledo Medical Center, Toledo, OH 43614, United States. FAU - Westrick, Judy AU - Westrick J AD - Department of Chemistry, College of Liberal Arts and Sciences, Wayne State University, Detroit, MI 48202, United States. FAU - Hensley, Kenneth AU - Hensley K AD - Department of Biochemistry, Cellular and Molecular Biology, Arkansas College of Osteopathic Medicine, Fort Smith, AR 72916, United States. FAU - Isailovic, Dragan AU - Isailovic D AD - Department of Chemistry and Biochemistry, College of Natural Sciences and Mathematics, University of Toledo, Toledo, OH 43606, United States. Electronic address: Dragan.Isailovic@utoledo.edu. LA - eng PT - Journal Article DEP - 20180817 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Microcystins) SB - IM MH - Animals MH - Blood Chemical Analysis/*methods MH - *Chromatography, High Pressure Liquid MH - Humans MH - Mice MH - Microcystins/*blood/*urine MH - *Solid Phase Extraction MH - *Tandem Mass Spectrometry MH - Urinalysis/*methods OTO - NOTNLM OT - Biofluids OT - LC-MS OT - MS/MS OT - Microcystins OT - Quantification OT - Solid-phase extraction EDAT- 2018/09/12 06:00 MHDA- 2018/11/02 06:00 CRDT- 2018/09/12 06:00 PHST- 2018/03/29 00:00 [received] PHST- 2018/08/02 00:00 [revised] PHST- 2018/08/09 00:00 [accepted] PHST- 2018/09/12 06:00 [pubmed] PHST- 2018/11/02 06:00 [medline] PHST- 2018/09/12 06:00 [entrez] AID - S0021-9673(18)31026-4 [pii] AID - 10.1016/j.chroma.2018.08.023 [doi] PST - ppublish SO - J Chromatogr A. 2018 Oct 26;1573:66-77. doi: 10.1016/j.chroma.2018.08.023. Epub 2018 Aug 17.