Ion Mobility Spectrometry in Food Analysis: Principles, Current Applications and Future Trends

In the last decade, ion mobility spectrometry (IMS) has reemerged as an analytical separation technique, especially due to the commercialization of ion mobility mass spectrometers. Its applicability has been extended beyond classical applications such as the determination of chemical warfare agents and nowadays it is widely used for the characterization of biomolecules (e.g., proteins, glycans, lipids, etc.) and, more recently, of small molecules (e.g., metabolites, xenobiotics, etc.). Following this trend, the interest in this technique is growing among researchers from different fields including food science. Several advantages are attributed to IMS when integrated in traditional liquid chromatography (LC) and gas chromatography (GC) mass spectrometry (MS) workflows: (1) it improves method selectivity by providing an additional separation dimension that allows the separation of isobaric and isomeric compounds; (2) it increases method sensitivity by isolating the compounds of interest from background noise; (3) and it provides complementary information to mass spectra and retention time, the so-called collision cross section (CCS), so compounds can be identified with more confidence, either in targeted or non-targeted approaches. In this context, the number of applications focused on food analysis has increased exponentially in the last few years. This review provides an overview of the current status of IMS technology and its applicability in different areas of food analysis (i.e., food composition, process control, authentication, adulteration and safety).M.H.-M. was granted a postdoctoral fellowship (University Research Plan, Program “Perfeccionamiento de doctores en el extranjero 2017”) by the University of Granada (Spain)

Multidimensional NMR approaches towards highly resolved, sensitive and high-throughput quantitative metabolomics

International audienceMulti-dimensional NMR is an appealing approach for dealing with the challenging complexity of biological samples in metabolomics. This article describes how spectroscopists have recently challenged their imagination in order to make 2D NMR a powerful tool for quantitative metabolomics, based on innovative pulse sequences combined with meticulous analytical chemistry approaches. Clever time-saving strategies have also been explored to make 2D NMR a high-throughput tool for metabolomics, relying on alternative data acquisition schemes such as ultrafast NMR. Currently, much work is aimed at drastically boosting the NMR sensitivity thanks to hyperpolarisation techniques, which have been used in combination with fast acquisition methods and could greatly expand the application potential of NMR metabolomics

Basics of mass spectrometry based metabolomics

International audienceThe emerging field of metabolomics, aiming to characterize small molecule metabolites present in biological systems, promises immense potential for different areas such as medicine, environmental sciences, agronomy, etc. The purpose of this article is to guide the reader through the history of the field, then through the main steps of the metabolomics workflow, from study design to structure elucidation, and help the reader to understand the key phases of a metabolomics investigation and the rationale underlying the protocols and techniques used. This article is not intended to give standard operating procedures as several papers related to this topic were already provided, but is designed as a tutorial aiming to help beginners understand the concept and challenges of MS-based metabolomics. A real case example is taken from the literature to illustrate the application of the metabolomics approach in the field of doping analysis. Challenges and limitations of the approach are then discussed along with future directions in research to cope with these limitations. This tutorial is part of the International Proteomics Tutorial Programme (IPTP18)

Selective androgen receptor modulators: comparative excretion study of bicalutamide in bovine urine and faeces

Besides their development for therapeutic purposes, non-steroidal selective androgen receptormodulators (non-steroidal SARMs) are also known to impact growth-associated pathways as ligands of androgenic receptors (AR). They present a potential for abuse in sports and food-producing animals as an interesting alternative to anabolic androgenic steroids (AAS). These compounds are easily available and could therefore be (mis)used in livestock production as growth promoters. To prevent such practices, dedicated analytical strategies should be developed for specific and sensitive detection of these compounds in biological matrices. The present study focused on Bicalutamide, a non-steroidal SARM used in human treatment of non-metastatic prostate cancer because of its anti-androgenic activity exhibiting no anti-anabolic effects. To select the most appropriate matrix to be used for control purposes, different animalmatrices (urine and faeces) have been investigated and SARM metabolism studied to highlight relevant metabolites of such treatments and establish associated detection time windows. The aim of this work was thus to compare the urinary and faecal eliminations of bicalutamide in a calf, and investigate phase I and II metabolites. The results in both matrices showed that bicalutamide was very rapidly and mainly excreted under its free form. The concentration levels were observed as higher in faeces (ppm) than urine (ppb); although both matrices were assessed as suitable for residue control. The metabolites found were consistent with hydroxylation (phase I reaction) combined or not with glucuronidation and sulfation (phase II reactions)Instituto de Tecnología de AlimentosFil: Sancho, Rojas, Dante Emanuel. Instituto Nacional de Tecnología Agropecuaria (INTA). Instituto de Tecnología de Alimentos, Argentina. LUNAM Université. Oniris, Laboratoire d’Etude des Résidus et Contaminants dans les Aliments; Francia.Fil: Dervilly-Pinel, Gaud. LUNAM Université. Oniris, Laboratoire d’Etude des Résidus et Contaminants dans les Aliments; Francia.Fil: Cesbron, Nora. LUNAM Université. Oniris, Laboratoire d’Etude des Résidus et Contaminants dans les Aliments; Francia.Fil: Penot, Mylène. LUNAM Université. Oniris, Laboratoire d’Etude des Résidus et Contaminants dans les Aliments; Francia.Fil: Sydor, Alexandre. LUNAM Université. Oniris, Laboratoire d’Etude des Résidus et Contaminants dans les Aliments; Francia.Fil: Prévost, Stéphanie. LUNAM Université. Oniris, Laboratoire d’Etude des Résidus et Contaminants dans les Aliments; Francia.Fil: Le Bizec, Bruno. LUNAM Université. Oniris, Laboratoire d’Etude des Résidus et Contaminants dans les Aliments; Francia

Urinary signature of pig carcasses with boar taint by liquid chromatography-high resolution mass spectrometry

Boar taint is an offensive odor that can occur while cooking pork or pork products and is identified in some uncastrated male pigs that have reached puberty. It is widely held that boar taint is the result of the accumulation in back-fat of two malodorous compounds: androstenone and skatole. The purpose of the present study was to assess a mass spectrometry-based metabolomics strategy to investigate the metabolic profile of urine samples from pig carcasses presenting low (untainted) and high (tainted) levels of androstenone and skatole in back fat. Urine samples were analyzed by LC-ESI(+)-HRMS. Discrimination between tainted and untainted animals was observed by application of multivariate statistical analysis, which allowed to highlight candidate urinary biomarkers. These urinary metabolites were positively correlated to androstenone and skatole levels in back fat. Therefore, the present study suggested that the measurement of these urinary metabolites might provide information with regard to androstenone and skatole levels in live pigs

Determination of a Large Set of β‑Adrenergic Agonists in Animal Matrices Based on Ion Mobility and Mass Separations

While the coupling of traveling wave ion mobility spectrometry (TWIMS) and mass spectrometry is mainly reported for structural purposes, we studied its potential in enhancing compounds analysis such as growth promoters used in livestock animals at trace concentrations. β-Adrenergic agonists have been selected as model compounds since they exhibit a range of close physicochemical properties leading to analytical issues using classical approaches. In this paper, the potential of Synapt G2-S (Q-TWIM-TOF MS) has been investigated for sensitive and specific detection of a range of these synthetic phenethanolamines in various complex biological matrices (retina, meat, and urine) from bovine considered as relevant in the context of detecting β-adrenergic agonists use in animals. In particular, the specificity of the additional information provided by the TWIMS (i.e., collision cross section) together with the interest of the extra dimension of separation is discussed