High resolution mass spectrometry workflow for the analysis of food contaminants: Application to plant toxins, mycotoxins and phytoestrogens in plant-based ingredients

A sensitive LC–MS/MS method for isomer separation and quantitative determination of 51 pyrrolizidine alkaloids and two tropane alkaloids in cow’s milk

“…To the best of our knowledge, sufficient resolution of all five isomers was so far only reported in a study using a 2D-LC setup [45]. Therefore, some authors conclude to reanalyse samples with a complementary RP-HPLC approach under different pH conditions or a HILIC method if inseparable PA/PANO were detected with the initially used LC method [32,34,41]. While the isomer pairs rinderine-N-oxide and echinatine-N-oxide and indicine-N-oxide and lycopsamine-N-oxide remained inseparable under the presented alkaline solvent conditions, they were separated by the tested acidic method, however co-eluting with other isomers instead [29].…”

“…Chromatographic resolution is especially crucial for the differentiation of the isomeric monoesters intermedine, indicine, lycopsamine, rinderine, and echinatine (m/z 300) and their N-oxides (m/z 316) as well as the cyclic diesters integerrimine, senecionine, and senecivernine (m/z 336) and their N-oxides (m/z 352), which were all included in the method development. In literature, mainly LC-MS/MS methods in reversed phase (RP) mode using C18 columns combined with both acidic or alkaline solvent conditions were reported for PA/PANO/TA analysis, with the latter solvent conditions being less common [29][30][31][32][33][34][35][36][37][38][39][40][41]. Only few methods were published using pentafluorophenyl (PFP) or hydrophilic interaction liquid chromatography (HILIC) columns [34,42,43].…”

“…The presented method was capable to achieve good sensitivity and separation for most of the critical isomeric pairs out of a large set of 56 PA/PANO analytes on a standard HPLC system within a run time of 31 min (including reequilibration). Recently published multi-PA/PANO methods mainly used ultra high-performance liquid chromatography (UHPLC) systems resulting in short run times of 11 to 25 min [32,34,37,41,44]. However, most of the methods published before did not include as many compounds from the isomeric group consisting of intermedine, indicine, lycopsamine, echinatine, and rinderine or their N-oxides, respectively.…”

Regulated and Non-Regulated Mycotoxin Detection in Cereal Matrices Using an Ultra-High-Performance Liquid Chromatography High-Resolution Mass Spectrometry (UHPLC-HRMS) Method

“…Furthermore, EFSA recently launched (February 2021) a call for data collection of chemical contaminants occurrence in the food chain, including ergot alkaloids (https://www.efsa.europa.eu/en/ call/call-continuous-collection-chemical-contaminants-occurrence-data-0, last accessed 11 October 2021). Worthy to notice is that although LC-HRMS methods for mycotoxin analysis in cereals were earlier published (see Introduction), they either did not target all the ergot alkaloids considered for EU regulations [22,23] or their detectability was worse [24] in comparison to the presented study. In fact, excellent analytical performance was achieved for all the analytes (see Section 2.1) and the method trueness was further demonstrated by analyzing the proficiency testing (PT) samples, attaining successful results.…”

Application of the QuEChERS Strategy as a Useful Sample Preparation Tool for the Multiresidue Determination of Pyrrolizidine Alkaloids in Food and Feed Samples: A Critical Overview

“…), pesticides, mycotoxins, drugs, phytoestrogens, etc. [19,23,[29][30][31][32][33][34][35]. However, despite its advantageous properties, the QuEChERS procedure has been scarcely employed for the analysis of PAs compared to SPE, as previously mentioned (Figure 1).…”