PMID- 31323558 OWN - NLM STAT- MEDLINE DCOM- 20191211 LR - 20191217 IS - 1873-376X (Electronic) IS - 1570-0232 (Linking) VI - 1125 DP - 2019 Sep 1 TI - Simultaneous determination of eight microcystins in fish by PRiME pass-through cleanup and online solid phase extraction coupled to ultra high performance liquid chromatography-tandem mass spectrometry. PG - 121709 LID - S1570-0232(19)30514-8 [pii] LID - 10.1016/j.jchromb.2019.06.036 [doi] AB - A rapid and sensitive method was developed based on online solid phase extraction coupled to ultra high performance liquid chromatography-tandem mass spectrometry (online SPE-UHPLC-MS/MS) for the simultaneous determination of eight common microcystins (MCs) in fish. Analytes, including MC-LR, MC-RR, MC-LY, MC-LW, MC-YR, MC-WR, MC-LF and MC-LA, were extracted by the solvent of MeOH: water (80:20, v/v) with 0.1% FA, and the extracted solution was cleaned up by one-step PRiME (process, robustness, improvements, matrix effects, ease of use) procedure before online SPE-UHPLC-MS/MS analysis. After the optimization of sample pretreatment conditions and instrumental parameters, method validation experiments were carried out to evaluate the performance of the method Good linearities were obtained in the range of 0.5-20 mug/L with r(2) larger than 0.99. The average recoveries of eight MCs spiked at 2, 10 and 20 mug/kg in fish samples were from 70.5% to 98.9% with relative standard deviations (RSDs) 1.3%-3.5% for repeatability and 2.2%-7.3% for reproducibility. Limits of detections (LODs) were ranged from 0.1 to 0.5 mug/kg and Limits of quantifications (LOQs) were in the range of 0.3-1.5 mug/kg. The developed method was further applied to the analysis of fish samples collected from Lake Taihu, China. MC-LR, MC-YR and MC-RR were detected in the range of 0.5-3.1 mug/kg. The experimental results proved the feasibility of the developed method for the identification and quantification of various MCs in fish products. CI - Copyright (c) 2019 Elsevier B.V. All rights reserved. FAU - Xu, Xiaoying AU - Xu X AD - Zhejiang Institute for Food and Drug Control, Hangzhou 310000, China. Electronic address: net_easexxy@126.com. FAU - Zhu, Bingqi AU - Zhu B AD - College of Medical Technology, Zhejiang Chinese Medical University, Hangzhou 310000, China. FAU - Liu, Zhu AU - Liu Z AD - Zhejiang Institute for Food and Drug Control, Hangzhou 310000, China. FAU - Wang, Feng AU - Wang F AD - Zhejiang Institute for Food and Drug Control, Hangzhou 310000, China. FAU - Liang, Jingjing AU - Liang J AD - Zhejiang Institute for Food and Drug Control, Hangzhou 310000, China. LA - eng PT - Evaluation Study PT - Journal Article DEP - 20190710 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 (Microcystins) RN - 77238-39-2 (microcystin) SB - IM MH - Animals MH - China MH - Chromatography, High Pressure Liquid/*methods MH - Fishes MH - Food Contamination/analysis MH - Limit of Detection MH - Microcystins/*chemistry/*isolation & purification MH - Seafood/analysis MH - Solid Phase Extraction/*methods MH - Tandem Mass Spectrometry/*methods OTO - NOTNLM OT - Fish OT - Microcystins OT - Online SPE-UHPLC-MS/MS OT - PRiME EDAT- 2019/07/20 06:00 MHDA- 2019/12/18 06:00 CRDT- 2019/07/20 06:00 PHST- 2019/03/27 00:00 [received] PHST- 2019/06/23 00:00 [revised] PHST- 2019/06/27 00:00 [accepted] PHST- 2019/07/20 06:00 [pubmed] PHST- 2019/12/18 06:00 [medline] PHST- 2019/07/20 06:00 [entrez] AID - S1570-0232(19)30514-8 [pii] AID - 10.1016/j.jchromb.2019.06.036 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Sep 1;1125:121709. doi: 10.1016/j.jchromb.2019.06.036. Epub 2019 Jul 10.