Analysis of Trace Microcystins in Vegetables Using Solid-Phase Extraction Followed by High Performance Liquid Chromatography Triple-Quadrupole Mass Spectrometry

Abstract

A selective and sensitive method for the simultaneous detection of three common and hazardous microcystins (microcystins-LR, -RR, and -YR) in various vegetables was established using solid-phase extraction followed by high performance liquid chromatography coupled with mass spectrometry. The methanol-water proportion ratio of the extraction solvent and its acidity, as well as the efficiencies of solid-phase extraction, were evaluated to optimize a pretreatment procedure for extracting the microcystins from 10 vegetable matrices. The limits of detection and quantitation were below 7.5 μg/kg (dw) and 25 μg/kg (dw), respectively, in different vegetable matrices. The recoveries of the microcystins in the 10 vegetable matrices ranged from 61.3 to 117.3%, with RSDs of 0.2-18.3%. The established method was used to analyze 28 field vegetable samples collected from the sides of Lake Dianchi, and microcystin-RR was found in almost all samples at concentrations of 36.4-2352.2 μg/kg (dw).

Double-sided magnetic molecularly imprinted polymer modified graphene oxide for highly efficient enrichment and fast detection of trace-level microcystins from large-volume water samples combined with liquid chromatography–tandem mass spectrometry

“…[13,14] . Today, MCs are of particular health concern as they are contaminants of sea foods, vegetables, and drinking water industries [15] , thus, the World Health Organization (WHO) recommends a Page 3 of 17 A c c e p t e d M a n u s c r i p 3 threshold limit of 1.0 µg·L -1 MC-LR in drinking water [16] . Therefore, a rapid, sensitive, and accurate analytical method is of particular importance for the determination of MCs in environmental water samples.…”

Cyanobacterial Toxins Emerging Contaminants in Soils: A Review of Sources, Fate and Impacts on Ecosystems, Plants and Animal and Human Health

“…For example, Järvenpää et al [138] reported that microcystins were detected on roots (a non-edible plant tissue for human but can be for animal) but not detected in leaves of mustard and broccoli. Furthermore, numerous studies concerning accumulation of cyanotoxins in agronomic plants growing in the soil were reported in radish roots, leaves of arugula and dill [61], in rice grains [65], in leaves of lettuce and cabbage [61,139], in leaves and stems of water spinach [139] and in fruits and seeds of tomato and pepper [64]. However, a recent study based on the use of 14 C-labelled MC-LR showed that tomato fruits did not accumulate the toxin [92].…”

New Method for Simultaneous Determination of Microcystins and Cylindrospermopsin in Vegetable Matrices by SPE-UPLC-MS/MS

“…Among these cyanotoxins, microcystins (MCs) and cylindrospermopsin (CYN) are amongst the most studied because of their widespread distribution. MCs, mainly produced by Microcystis , have the common cyclic heptapeptidic structure of cyclo(- d -Ala- l -X- d -MeAsp- l -Z-Adda- d -Glu-Mdha), in which X and Z are variable l -amino acids that give the name to the molecule [ 4 ]. Because of these modifications, and the methylation/desmethylation of several functional groups, more than 100 MC variants have been reported to date [ 5 ].…”

“…On the other hand, CYN is an alkaloid consisting of a tricyclic guanidine moiety combined with hidroxymethiluracil, which can be produced by Cylindrospermopsis raciborskii and Chrysosporum ovalisporum [ 7 ]. Concerning the mechanism of action, MCs are hepatotoxins and tumor promoters due to their strong potent inhibition of protein phosphatases and the effect on cell signaling pathways [ 4 ]. CYN is well known by its inhibition of protein and glutathione synthesis, induction of oxidative stress, and cytochrome P450 seems to mediate its toxicity; its pro-genotoxic activity has also been studied [ 6 , 8 ].…”