Recent developments in sample-pretreatment techniques for mass spectrometry-based metabolomics

Abstract Metabolomics is one of the most rapidly evolving of the omics sciences. For phenotyping individuals, it offers a promising platform that is needed for breakthroughs in biomedical and pharmacological research. A proper sample-pretreatment procedure is required for metabolomics studies to overcome the mismatch of the sample with the analytical method. Within the analytical workflow for metabolomics studies, sample pretreatment is important in order to obtain the meaningful, high-quality quantitative data needed to minimize inconsistencies between laboratories. In this review, we provide an overview of state-of-the-art sample-pretreatment techniques for mass spectrometry-based metabolomics. We pay attention to deproteinization, removal of interfering molecules, liquid-liquid extraction, solid-phase extraction, electromigration-based extraction methods and possibly emerging sample-pretreatment techniques for metabolomics. We give the advantages and the limitations of these techniques for metabolomics, and consider aspects such as automation and high-throughput analysis. Finally, we provide some conclusions and perspectives.

[1]  R. Krska,et al.  Isotopic labeling-assisted metabolomics using LC–MS , 2012, Analytical and Bioanalytical Chemistry.

[2]  J. Keiser,et al.  Systematic Evaluation of Extraction Methods for Multiplatform-Based Metabotyping: Application to the Fasciola hepatica Metabolome , 2012, Analytical chemistry.

[3]  M. Karas,et al.  Effect of different solution flow rates on analyte ion signals in nano-ESI MS, or: when does ESI turn into nano-ESI? , 2003, Journal of the American Society for Mass Spectrometry.

[4]  Catherine A Rimmer,et al.  Development of a Standard Reference Material for metabolomics research. , 2013, Analytical chemistry.

[5]  M. D. Luque de Castro,et al.  Metabolomics analysis I. Selection of biological samples and practical aspects preceding sample preparation , 2010 .

[6]  Y. Yamini,et al.  Electrical field-induced extraction and separation techniques: promising trends in analytical chemistry--a review. , 2014, Analytica chimica acta.

[7]  Y Wang,et al.  Targeted metabolomics and mass spectrometry. , 2010, Advances in protein chemistry and structural biology.

[8]  Ian D Wilson,et al.  Hydrophilic interaction and reversed-phase ultra-performance liquid chromatography TOF-MS for metabonomic analysis of Zucker rat urine. , 2008, Journal of separation science.

[9]  R. Goodacre,et al.  Metabolite extraction from suspension-cultured mammalian cells for global metabolite profiling , 2011, Nature Protocols.

[10]  A. Cifuentes,et al.  CE/LC‐MS multiplatform for broad metabolomic analysis of dietary polyphenols effect on colon cancer cells proliferation , 2012, Electrophoresis.

[11]  D. Fast,et al.  Systematic evaluation of supported liquid extraction in reducing matrix effect and improving extraction efficiency in LC-MS/MS based bioanalysis for 10 model pharmaceutical compounds. , 2012, Journal of chromatography. B, Analytical technologies in the biomedical and life sciences.

[12]  J. Kreuder,et al.  Metabonomics of newborn screening dried blood spot samples: a novel approach in the screening and diagnostics of inborn errors of metabolism. , 2012, Analytical chemistry.

[13]  Liang Li,et al.  Liquid-liquid extraction combined with differential isotope dimethylaminophenacyl labeling for improved metabolomic profiling of organic acids. , 2013, Analytica chimica acta.

[14]  Jerzy Adamski,et al.  Procedure for tissue sample preparation and metabolite extraction for high-throughput targeted metabolomics , 2011, Metabolomics.

[15]  Michael Vogeser,et al.  Deproteination of serum samples for LC-MS/MS analyses by applying magnetic micro-particles. , 2013, Clinical biochemistry.

[16]  S. Inokuchi,et al.  Monolithic spin column extraction and GC-MS for the simultaneous assay of diquat, paraquat, and fenitrothion in human serum and urine , 2011, Analytical and bioanalytical chemistry.

[17]  J. Pawliszyn,et al.  Silica-based ionic liquid coating for 96-blade system for extraction of aminoacids from complex matrixes. , 2013, Analytica chimica acta.

[18]  Coral Barbas,et al.  In-vial dual extraction for direct LC-MS analysis of plasma for comprehensive and highly reproducible metabolic fingerprinting. , 2012, Analytical chemistry.

[19]  R. Chang,et al.  Metabolic phenotype of the healthy rodent model using in-vial extraction of dried serum, urine, and cerebrospinal fluid spots. , 2013, Analytical chemistry.

[20]  Thomas Hankemeier,et al.  The influence of citrate, EDTA, and heparin anticoagulants to human plasma LC–MS lipidomic profiling , 2012, Metabolomics.

[21]  J. Rabinowitz,et al.  Metabolomics in drug target discovery. , 2011, Cold Spring Harbor symposia on quantitative biology.

[22]  V. Pichon,et al.  Novel extraction supports based on immobilised aptamers: evaluation for the selective extraction of cocaine. , 2011, Talanta.

[23]  Fabian J Theis,et al.  The dynamic range of the human metabolome revealed by challenges , 2012, FASEB journal : official publication of the Federation of American Societies for Experimental Biology.

[24]  Stephen J. Bruce,et al.  Investigation of human blood plasma sample preparation for performing metabolomics using ultrahigh performance liquid chromatography/mass spectrometry. , 2009, Analytical chemistry.

[25]  N. Spooner,et al.  The effect of hematocrit and punch location on assay bias during quantitative bioanalysis of dried blood spot samples. , 2011, Bioanalysis.

[26]  A. Cifuentes,et al.  Is metabolomics reachable? Different purification strategies of human colon cancer cells provide different CE‐MS metabolite profiles , 2011, Electrophoresis.

[27]  Robert S Plumb,et al.  Global metabolic profiling of animal and human tissues via UPLC-MS , 2012, Nature Protocols.

[28]  Frank Suits,et al.  The impact of delayed storage on the measured proteome and metabolome of human cerebrospinal fluid. , 2011, Clinical chemistry.

[29]  S. Gatzek,et al.  Controlled protein precipitation in combination with chip-based nanospray infusion mass spectrometry. An approach for metabolomics profiling of plasma. , 2005, Analytical chemistry.

[30]  U. Sauer,et al.  Cross-platform comparison of methods for quantitative metabolomics of primary metabolism. , 2009, Analytical chemistry.

[31]  Joshua D. Knowles,et al.  Procedures for large-scale metabolic profiling of serum and plasma using gas chromatography and liquid chromatography coupled to mass spectrometry , 2011, Nature Protocols.

[32]  T. Hankemeier,et al.  Three-phase electroextraction: a new (online) sample purification and enrichment method for bioanalysis. , 2013, Analytical chemistry.

[33]  M. Armstrong,et al.  New sample preparation approach for mass spectrometry-based profiling of plasma results in improved coverage of metabolome. , 2013, Journal of chromatography. A.

[34]  Á. Ravelo,et al.  Dichloromethane as a solvent for lipid extraction and assessment of lipid classes and fatty acids from samples of different natures. , 2008, Journal of agricultural and food chemistry.

[35]  Gordana Ivosev,et al.  Comprehensive analytical strategy for biomarker identification based on liquid chromatography coupled to mass spectrometry and new candidate confirmation tools. , 2009, Analytical chemistry.

[36]  Takeshi Saito,et al.  Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection. , 2010, Analytica chimica acta.

[37]  R. Perestrelo,et al.  Re-exploring the high-throughput potential of microextraction techniques, SPME and MEPS, as powerful strategies for medical diagnostic purposes. Innovative approaches, recent applications and future trends , 2014, Analytical and Bioanalytical Chemistry.

[38]  E. Want,et al.  Global metabolic profiling procedures for urine using UPLC–MS , 2010, Nature Protocols.

[39]  Joshua LaBaer,et al.  Improving international research with clinical specimens: 5 achievable objectives. , 2012, Journal of proteome research.

[40]  I. Wilson,et al.  Metabolite profiles from dried biofluid spots for metabonomic studies using UPLC combined with oaToF-MS. , 2010, Journal of proteome research.

[41]  P. Britz‐McKibbin,et al.  Comprehensive plasma thiol redox status determination for metabolomics. , 2011, Journal of proteome research.

[42]  G. Theodoridis,et al.  Sample preparation prior to the LC-MS-based metabolomics/metabonomics of blood-derived samples. , 2011, Bioanalysis.

[43]  Georgios Theodoridis,et al.  UPLC-MS-based analysis of human plasma for metabonomics using solvent precipitation or solid phase extraction. , 2009, Journal of proteome research.

[44]  S. Wilson,et al.  On-line solid phase extraction-liquid chromatography, with emphasis on modern bioanalysis and miniaturized systems. , 2014, Journal of pharmaceutical and biomedical analysis.

[45]  W. J. Dyer,et al.  A rapid method of total lipid extraction and purification. , 1959, Canadian journal of biochemistry and physiology.

[46]  G. Fan,et al.  Development and validation of a rapid and high-sensitivity liquid chromatography-tandem mass spectrometry assay for the determination of neostigmine in small-volume beagle dog plasma and its application to a pharmacokinetic study. , 2014, Biomedical chromatography : BMC.

[47]  T. Hankemeier,et al.  Quantitative profiling of oxylipins through comprehensive LC-MS/MS analysis: application in cardiac surgery , 2012, Analytical and Bioanalytical Chemistry.

[48]  S. Pedersen‐Bjergaard,et al.  Electrokinetic migration across artificial liquid membranes. New concept for rapid sample preparation of biological fluids. , 2006, Journal of chromatography. A.

[49]  G. Siuzdak,et al.  Expanding coverage of the metabolome for global metabolite profiling. , 2011, Analytical chemistry.

[50]  Amirhassan Amiri,et al.  Liquid-phase microextraction , 2010 .

[51]  Semiautomated Device for Batch Extraction of Metabolites from Tissue Samples , 2012, Analytical chemistry.

[52]  E. Want,et al.  Cross-platform comparison of Caenorhabditis elegans tissue extraction strategies for comprehensive metabolome coverage. , 2011, Analytical chemistry.

[53]  M. D. Luque de Castro,et al.  Ultrasound: a subexploited tool for sample preparation in metabolomics. , 2014, Analytica chimica acta.

[54]  T. Hankemeier,et al.  Online capillary liquid–liquid electroextraction of peptides as fast pre‐concentration prior to LC‐MS , 2010, Electrophoresis.

[55]  M. Vogeser,et al.  Progress in automation of LC-MS in laboratory medicine. , 2011, Clinical biochemistry.

[56]  O. Fiehn Metabolomics – the link between genotypes and phenotypes , 2004, Plant Molecular Biology.

[57]  Joseph A Tweed,et al.  Automated supported liquid extraction using 2D barcode processing for routine toxicokinetic portfolio support. , 2012, Bioanalysis.

[58]  B. McManus,et al.  The Human Serum Metabolome , 2011, PloS one.

[59]  P. Boček,et al.  Electromembrane extraction of amino acids from body fluids followed by capillary electrophoresis with capacitively coupled contactless conductivity detection. , 2011, Journal of chromatography. A.

[60]  Richard D. Beger,et al.  A Review of Applications of Metabolomics in Cancer , 2013, Metabolites.

[61]  T. Hankemeier,et al.  Feasibility of electroextraction as versatile sample preconcentration for fast and sensitive analysis of urine metabolites, demonstrated on acylcarnitines , 2012, Electrophoresis.

[62]  I. Wilson Global metabolic profiling (metabonomics/metabolomics) using dried blood spots: advantages and pitfalls. , 2011, Bioanalysis.

[63]  Erik Peter,et al.  Quality markers addressing preanalytical variations of blood and plasma processing identified by broad and targeted metabolite profiling. , 2014, Clinical chemistry.

[64]  I. Wilson,et al.  Application of turbulent flow chromatography to the metabonomic analysis of human plasma: comparison with protein precipitation. , 2010, Journal of separation science.

[65]  T. Hankemeier,et al.  Quantitative metabolomics based on gas chromatography mass spectrometry: status and perspectives , 2010, Metabolomics.

[66]  A. Furey,et al.  Ion suppression; a critical review on causes, evaluation, prevention and applications. , 2013, Talanta.

[67]  Rainer Bischoff,et al.  Chemical and technical challenges in the analysis of central carbon metabolites by liquid-chromatography mass spectrometry. , 2014, Journal of chromatography. B, Analytical technologies in the biomedical and life sciences.

[68]  J. Santiago-García,et al.  Saliva: a fluid of study for OMICS. , 2014, Omics : a journal of integrative biology.

[69]  Coral Barbas,et al.  In-vial dual extraction liquid chromatography coupled to mass spectrometry applied to streptozotocin-treated diabetic rats. Tips and pitfalls of the method. , 2013, Journal of chromatography. A.

[70]  C. Burant,et al.  Reducing time and increasing sensitivity in sample preparation for adherent mammalian cell metabolomics. , 2011, Analytical chemistry.

[71]  R. Dixon,et al.  Development of isotope labeling LC-MS for human salivary metabolomics and application to profiling metabolome changes associated with mild cognitive impairment. , 2012, Analytical chemistry.

[72]  E. Schleicher,et al.  Simultaneous extraction of metabolome and lipidome with methyl tert-butyl ether from a single small tissue sample for ultra-high performance liquid chromatography/mass spectrometry. , 2013, Journal of chromatography. A.

[73]  T. Hyötyläinen Critical evaluation of sample pretreatment techniques , 2009, Analytical and bioanalytical chemistry.

[74]  J. Folch,et al.  A simple method for the isolation and purification of total lipides from animal tissues. , 1957, The Journal of biological chemistry.

[75]  D. Neville,et al.  Efficacy of plasma phospholipid removal during sample preparation and subsequent retention under typical UHPLC conditions. , 2012, Bioanalysis.

[76]  Á. Gil-Izquierdo,et al.  Metabolomics and the diagnosis of human diseases--a guide to the markers and pathophysiological pathways affected. , 2014, Current medicinal chemistry.

[77]  G. Siuzdak,et al.  Solvent-dependent metabolite distribution, clustering, and protein extraction for serum profiling with mass spectrometry. , 2006, Analytical chemistry.

[78]  T. Hankemeier,et al.  The potential of electrophoretic sample pretreatment techniques and new instrumentation for bioanalysis, with a focus on peptidomics and metabolomics. , 2013, Bioanalysis.

[79]  D. Vuckovic Current trends and challenges in sample preparation for global metabolomics using liquid chromatography–mass spectrometry , 2012, Analytical and Bioanalytical Chemistry.

[80]  K. G. Prasad,et al.  Diatomaceous earth supported liquid extraction and LC-MS/MS determination of elvitegravir and ritonavir in rat plasma: application to a pharmacokinetic study , 2013 .