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A new class of foreign substances present in the unsaponifiable fraction of vegetable oils undergone to chemical interesterification was systematically investigated. Their chemical structure, corresponding to dialkyl ketones (DAK) molecules, was elucidated both by gas chromatography-mass spectrometry (GC-MS), and liquid chromatography-high resolution mass spectrometry (LC-HRMS). An analytical protocol aimed to qualitative and quantitative detection of DAK molecules in vegetable oils of confectionery industry interest was developed. Being the range of concentration levels to be evaluated dependent on the technological task of interesterification process, the quantitation step was thoroughly examined. All the validation parameters were satisfactory and particularly the concentration determinations were made more reliable by the contemporary use of several quantitation standards. GC-MS and LC-HRMS analytical techniques exhibited comparable performances even if the second one shown better detection sensitivity., (Copyright © 2018 Elsevier B.V. All rights reserved.)

The analysis of lipid molecules in living organism is an important step in deciphering metabolic pathways. Recently, the zebrafish has been adopted as a valuable animal model system to perform in vivo metabolomics studies, however limited methodologies and protocols are currently available to investigate zebrafish lipidome and even fewer to analyze specific classes of lipids. Here we present an HPLC-HRMS based method to rapidly measure multiple prenol lipid molecules from zebrafish tissues. In particular, we have optimized our method for concurrent detection of ubiquinones (Coenzyme Q6, Coenzyme Q9, Coenzyme Q10), cholesterol, vitamin E (α-tocopherol), vitamin K1 and vitamin K2. The purpose of this study was to compare different ionization modes, mobile phases and stationary phases in order to optimize lipid molecules separation. After HPLC-HRMS parameters selection, several extraction conditions from zebrafish embryos were evaluated. We assessed our methodology by quantitation of analytical recovery on zebrafish extracts from wild-type or zebrafish mutants (barolo) affected by impaired biosynthesis of ubiquinones., (Copyright © 2015 Elsevier B.V. All rights reserved.)

High-performance liquid chromatography coupled to ultraviolet diode array detection and electrospray ionization mass spectrometry was applied to monitor the photocatalytic degradation mediated by TiO2 of three sulfonated monoazo dyes (Orange I, Orange II, and Ethylorange) present in aqueous solution. Photobleaching, organic carbon, nitrogen and sulfur evolution were also followed during the process. Delayed carbon mineralization was observed with respect to both dyes disappearance and photobleaching, due to the formation of transient intermediate compounds which were in turn completely degraded. Among the intermediates produced during the initial degradation steps the formation of several hydroxylated derivatives, mostly coloured, was evidenced. The MS(2) spectra allowed one to formulate hypothesis about the OH attack positions; a peculiar reactivity of the azo moiety was shown by Orange I and Orange II.