Biomaterial Database

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. 2019

Xiaoying Xu, and Bingqi Zhu, and Zhu Liu, and Feng Wang, and Jingjing Liang

Zhejiang Institute for Food and Drug Control, Hangzhou 310000, China. Electronic address: net_easexxy@126.com.

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 μg/L with r2 larger than 0.99. The average recoveries of eight MCs spiked at 2, 10 and 20 μg/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 μg/kg and Limits of quantifications (LOQs) were in the range of 0.3-1.5 μg/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 μg/kg. The experimental results proved the feasibility of the developed method for the identification and quantification of various MCs in fish products.

UI	MeSH Term	Description	Entries
D002681	China	A country spanning from central Asia to the Pacific Ocean.	Inner Mongolia,Manchuria,People's Republic of China,Sinkiang,Mainland China
D002851	Chromatography, High Pressure Liquid	Liquid chromatographic techniques which feature high inlet pressures, high sensitivity, and high speed.	Chromatography, High Performance Liquid,Chromatography, High Speed Liquid,Chromatography, Liquid, High Pressure,HPLC,High Performance Liquid Chromatography,High-Performance Liquid Chromatography,UPLC,Ultra Performance Liquid Chromatography,Chromatography, High-Performance Liquid,High-Performance Liquid Chromatographies,Liquid Chromatography, High-Performance
D005399	Fishes	A group of cold-blooded, aquatic vertebrates having gills, fins, a cartilaginous or bony endoskeleton, and elongated bodies covered with scales.
D005506	Food Contamination	The presence in food of harmful, unpalatable, or otherwise objectionable foreign substances, e.g. chemicals, microorganisms or diluents, before, during, or after processing or storage.	Food Adulteration,Adulteration, Food,Adulterations, Food,Contamination, Food,Contaminations, Food,Food Adulterations,Food Contaminations
D000818	Animals	Unicellular or multicellular, heterotrophic organisms, that have sensation and the power of voluntary movement. Under the older five kingdom paradigm, Animalia was one of the kingdoms. Under the modern three domain model, Animalia represents one of the many groups in the domain EUKARYOTA.	Animal,Metazoa,Animalia
D017747	Seafood	Marine fish and shellfish used as food or suitable for food. (Webster, 3d ed) SHELLFISH and FISH PRODUCTS are more specific types of SEAFOOD.	Sea-Food,Sea Food,Sea-Foods,Seafoods
D052616	Solid Phase Extraction	An extraction method that separates analytes using a solid phase and a liquid phase. It is used for preparative sample cleanup before analysis by CHROMATOGRAPHY and other analytical methods.	Extraction, Solid Phase,Extractions, Solid Phase,Solid Phase Extractions
D052998	Microcystins	Cyclic heptapeptides found in MICROCYSTIS and other CYANOBACTERIA. Hepatotoxic and carcinogenic effects have been noted. They are sometimes called cyanotoxins, which should not be confused with chemicals containing a cyano group (CN) which are toxic.	Cyanoginosins
D053719	Tandem Mass Spectrometry	A mass spectrometry technique using two (MS/MS) or more mass analyzers. With two in tandem, the precursor ions are mass-selected by a first mass analyzer, and focused into a collision region where they are then fragmented into product ions which are then characterized by a second mass analyzer. A variety of techniques are used to separate the compounds, ionize them, and introduce them to the first mass analyzer. For example, for in GC-MS/MS, GAS CHROMATOGRAPHY-MASS SPECTROMETRY is involved in separating relatively small compounds by GAS CHROMATOGRAPHY prior to injecting them into an ionization chamber for the mass selection.	Mass Spectrometry-Mass Spectrometry,Mass Spectrometry Mass Spectrometry,Mass Spectrometry, Tandem
D057230	Limit of Detection	Concentration or quantity that is derived from the smallest measure that can be detected with reasonable certainty for a given analytical procedure.	Limits of Detection,Detection Limit,Detection Limits