Plant metabolomics and its potential for systems biology research background concepts, technology, and methodology.

[1]  Dirk Walther,et al.  Progress in Chemometrics and Biostatistics for Plant Applications, or: A Good Red Wine is a Bad White Wine , 2011 .

[2]  Henning Redestig,et al.  Data Integration, Metabolic Networks and Systems Biology , 2011 .

[3]  O. Fiehn,et al.  Data Processing, Metabolomic Databases and Pathway Analysis , 2011 .

[4]  N. V. van Dam,et al.  A Role for Metabolomics in Plant Ecology , 2011 .

[5]  Michael R. Sussman,et al.  Metabolomics of Arabidopsis Thaliana , 2011 .

[6]  Robert D Hall,et al.  Plant molecular stress responses face climate change. , 2010, Trends in plant science.

[7]  M. Gromova,et al.  Toward Arabidopsis thaliana hydrophilic metabolome: assessment of extraction methods and quantitative 1H NMR. , 2010, Physiologia plantarum.

[8]  Guillaume L. Erny,et al.  Quantification of organic acids in beer by nuclear magnetic resonance (NMR)-based methods. , 2010, Analytica chimica acta.

[9]  Sonia J. Miller,et al.  The metabolic transition during disease following infection of Arabidopsis thaliana by Pseudomonas syringae pv. tomato. , 2010, The Plant journal : for cell and molecular biology.

[10]  Arjen Lommen,et al.  Ultra-fast searching assists in evaluating sub-ppm mass accuracy enhancement in U-HPLC/Orbitrap MS data , 2010, Metabolomics.

[11]  Robert D. Hall,et al.  Plant Metabolomics Applications in the Brassicaceae: Added Value for Science and Industry , 2010 .

[12]  Y. Choi,et al.  Metabolomics: a tool for anticancer lead-finding from natural products. , 2010, Planta medica.

[13]  M. Stitt,et al.  Mild reductions in cytosolic NADP-dependent isocitrate dehydrogenase activity result in lower amino acid contents and pigmentation without impacting growth , 2010, Amino Acids.

[14]  Kazuki Saito,et al.  Metabolomics for functional genomics, systems biology, and biotechnology. , 2010, Annual review of plant biology.

[15]  V. Gómez-Roldán,et al.  Strategies to Optimize the Flavonoid Content of Tomato Fruit , 2010 .

[16]  Royston Goodacre,et al.  Dual metabolomics: a novel approach to understanding plant-pathogen interactions. , 2010, Phytochemistry.

[17]  M. Udvardi,et al.  Mining for robust transcriptional and metabolic responses to long-term salt stress: a case study on the model legume Lotus japonicus. , 2010, Plant, cell & environment.

[18]  John M. Baker,et al.  An inter-laboratory comparison demonstrates that [1H]-NMR metabolite fingerprinting is a robust technique for collaborative plant metabolomic data collection , 2010, Metabolomics.

[19]  Joachim Selbig,et al.  Decision tree supported substructure prediction of metabolites from GC-MS profiles , 2010, Metabolomics.

[20]  R. Goodacre,et al.  Metabolic acclimation to hypoxia revealed by metabolite gradients in melon fruit. , 2010, Journal of plant physiology.

[21]  Jürgen Hartmann,et al.  Metabolic profiling of Arabidopsis thaliana epidermal cells , 2010, Journal of experimental botany.

[22]  J. Joyard,et al.  Plant Systems Biology , 2010, Plant Physiology.

[23]  C. Larive,et al.  A comparison of metabolite extraction strategies for 1H‐NMR‐based metabolic profiling using mature leaf tissue from the model plant Arabidopsis thaliana , 2009, Magnetic resonance in chemistry : MRC.

[24]  Ilya Venger,et al.  Fruit-Surface Flavonoid Accumulation in Tomato Is Controlled by a SlMYB12-Regulated Transcriptional Network , 2009, PLoS genetics.

[25]  Robert D Hall,et al.  A Role for Differential Glycoconjugation in the Emission of Phenylpropanoid Volatiles from Tomato Fruit Discovered Using a Metabolic Data Fusion Approach1[W][OA] , 2009, Plant Physiology.

[26]  B. Usadel,et al.  Xeml Lab: a tool that supports the design of experiments at a graphical interface and generates computer-readable metadata files, which capture information about genotypes, growth conditions, environmental perturbations and sampling strategy. , 2009, Plant, cell & environment.

[27]  Royston Goodacre,et al.  Inter-laboratory reproducibility of fast gas chromatography–electron impact–time of flight mass spectrometry (GC–EI–TOF/MS) based plant metabolomics , 2009, Metabolomics.

[28]  Joshua D. Knowles,et al.  Development and performance of a gas chromatography-time-of-flight mass spectrometry analysis for large-scale nontargeted metabolomic studies of human serum. , 2009, Analytical chemistry.

[29]  L. Willmitzer,et al.  13C isotope-labeled metabolomes allowing for improved compound annotation and relative quantification in liquid chromatography-mass spectrometry-based metabolomic research. , 2009, Analytical chemistry.

[30]  J. W. Allwood,et al.  1H NMR, GC-EI-TOFMS, and data set correlation for fruit metabolomics: application to spatial metabolite analysis in melon. , 2009, Analytical chemistry.

[31]  J. Keurentjes.  Genetical metabolomics: closing in on phenotypes. , 2009, Current opinion in plant biology.

[32]  Arjen Lommen,et al.  MetAlign: interface-driven, versatile metabolomics tool for hyphenated full-scan mass spectrometry data preprocessing. , 2009, Analytical chemistry.

[33]  J. J. Jansen,et al.  Metabolomic analysis of the interaction between plants and herbivores , 2009, Metabolomics.

[34]  Bernd Schneider,et al.  Plant micrometabolomics: the analysis of endogenous metabolites present in a plant cell or tissue. , 2009, Journal of proteome research.

[35]  Ilya Venger,et al.  Non-targeted analysis of spatial metabolite composition in strawberry (Fragariaxananassa) flowers. , 2008, Phytochemistry.

[36]  P. Kachlicki,et al.  Differentiation of isomeric malonylated flavonoid glyconjugates in plant extracts with UPLC-ESI/MS/MS. , 2008, Phytochemical analysis : PCA.

[37]  A. Fernie,et al.  Reconfiguration of the Achene and Receptacle Metabolic Networks during Strawberry Fruit Development1[C][W] , 2008, Plant Physiology.

[38]  Jan Hummel,et al.  Retention index thresholds for compound matching in GC-MS metabolite profiling. , 2008, Journal of chromatography. B, Analytical technologies in the biomedical and life sciences.

[39]  D. Kell,et al.  Metabolic profiling of serum using Ultra Performance Liquid Chromatography and the LTQ-Orbitrap mass spectrometry system. , 2008, Journal of chromatography. B, Analytical technologies in the biomedical and life sciences.

[40]  Kazuki Saito,et al.  Comprehensive Flavonol Profiling and Transcriptome Coexpression Analysis Leading to Decoding Gene–Metabolite Correlations in Arabidopsis[W][OA] , 2008, The Plant Cell Online.

[41]  R. Balestrini,et al.  Laser Microdissection (LM): Applications to plant materials , 2008 .

[42]  Peter J Oefner,et al.  Development of a quantitative, validated Capillary electrophoresis‐time of flight – mass spectrometry method with integrated high‐confidence analyte identification for metabolomics , 2008, Electrophoresis.

[43]  S. Kanaya,et al.  Metabolite annotations based on the integration of mass spectral information , 2008, The Plant journal : for cell and molecular biology.

[44]  Alexander Erban,et al.  TagFinder for the quantitative analysis of gas chromatography - mass spectrometry (GC-MS)-based metabolite profiling experiments , 2008, Bioinform..

[45]  Serge Rudaz,et al.  Optimized liquid chromatography-mass spectrometry approach for the isolation of minor stress biomarkers in plant extracts and their identification by capillary nuclear magnetic resonance. , 2008, Journal of chromatography. A.

[46]  Oliver Fiehn,et al.  Quality control for plant metabolomics: reporting MSI-compliant studies. , 2008, The Plant journal : for cell and molecular biology.

[47]  Jules Beekwilder,et al.  Changes in antioxidant and metabolite profiles during production of tomato paste. , 2008, Journal of agricultural and food chemistry.

[48]  E. Çapanoğlu,et al.  Tissue specialization at the metabolite level is perceived during the development of tomato fruit. , 2007, Journal of experimental botany.

[49]  R. Dixon,et al.  Metabolomics Reveals Novel Pathways and Differential Mechanistic and Elicitor-Specific Responses in Phenylpropanoid and Isoflavonoid Biosynthesis in Medicago truncatula Cell Cultures1[C][W][OA] , 2007, Plant Physiology.

[50]  Royston Goodacre,et al.  Metabolomic technologies and their application to the study of plants and plant-host interactions. , 2007, Physiologia plantarum.

[51]  Ute Roessner,et al.  Plant metabolomics reveals conserved and divergent metabolic responses to salinity. , 2007, Physiologia plantarum.

[52]  A. Fernie.  The future of metabolic phytochemistry: larger numbers of metabolites, higher resolution, greater understanding. , 2007, Phytochemistry.

[53]  Wolfgang Eisenreich,et al.  Advances of high-resolution NMR techniques in the structural and metabolic analysis of plant biochemistry. , 2007, Phytochemistry.

[54]  R. Bino,et al.  Metabolomics technologies and metabolite identification , 2007 .

[55]  Douglas B. Kell,et al.  Proposed minimum reporting standards for data analysis in metabolomics , 2007, Metabolomics.

[56]  Ute Roessner,et al.  Minimum reporting standards for plant biology context information in metabolomic studies , 2007, Metabolomics.

[57]  Yves Gibon,et al.  GC-EI-TOF-MS analysis of in vivo carbon-partitioning into soluble metabolite pools of higher plants by monitoring isotope dilution after 13CO2 labelling. , 2007, Phytochemistry.

[58]  Xiaosong Hu,et al.  The Effect of Freezing Modes and Frozen Storage on Aroma, Enzyme and Micro-organism in Hami Melon , 2007 .

[59]  J. Keurentjes,et al.  Untargeted large-scale plant metabolomics using liquid chromatography coupled to mass spectrometry , 2007, Nature Protocols.

[60]  Douglas B. Kell,et al.  Statistical strategies for avoiding false discoveries in metabolomics and related experiments , 2007, Metabolomics.

[61]  B. Mueller‐Roeber,et al.  Profiling of phenolic glycosidic conjugates in leaves of Arabidopsis thaliana using LC/MS , 2007, Metabolomics.

[62]  Danielle Ryan,et al.  Analytical Chemistry Considerations in Plant Metabolomics , 2006 .

[63]  Y. Choi,et al.  Metabolomic analysis of methyl jasmonate treated Brassica rapa leaves by 2-dimensional NMR spectroscopy. , 2006, Phytochemistry.

[64]  Yves Gibon,et al.  Integration of metabolite with transcript and enzyme activity profiling during diurnal cycles in Arabidopsis rosettes , 2006, Genome Biology.

[65]  P. Pieri,et al.  Microclimate influence on mineral and metabolic profiles of grape berries. , 2006, Journal of agricultural and food chemistry.

[66]  Jingyuan Fu,et al.  The genetics of plant metabolism , 2006, Nature Genetics.

[67]  A. Fernie,et al.  Gas chromatography mass spectrometry–based metabolite profiling in plants , 2006, Nature Protocols.

[68]  David I. Ellis,et al.  Metabolomic approaches reveal that phosphatidic and phosphatidyl glycerol phospholipids are major discriminatory non-polar metabolites in responses by Brachypodium distachyon to challenge by Magnaporthe grisea. , 2006, The Plant journal : for cell and molecular biology.

[69]  Jean-Marc Nuzillard,et al.  NMR metabolomics to revisit the tobacco mosaic virus infection in Nicotiana tabacum leaves. , 2006, Journal of natural products.

[70]  U. Roessner,et al.  Comprehensive metabolic profiling and phenotyping of interspecific introgression lines for tomato improvement , 2006, Nature Biotechnology.

[71]  Jörg-Peter Schnitzler,et al.  Practical approaches to plant volatile analysis. , 2006, The Plant journal : for cell and molecular biology.

[72]  G. Beecher,et al.  Stability of 5-methyltetrahydrofolate in frozen fresh fruits and vegetables , 2005 .

[73]  Klaus Albert,et al.  LC–NMR coupling technology: recent advancements and applications in natural products analysis , 2005, Magnetic resonance in chemistry : MRC.

[74]  Oliver Fiehn,et al.  Metabolic profiling of laser microdissected vascular bundles of Arabidopsis thaliana , 2005, Plant Methods.

[75]  Olivier Lavialle,et al.  1H NMR and chemometrics to characterize mature grape berries in four wine-growing areas in Bordeaux, France. , 2005, Journal of agricultural and food chemistry.

[76]  R. Bino,et al.  The light-hyperresponsive high pigment-2dg mutation of tomato: alterations in the fruit metabolome. , 2005, The New phytologist.

[77]  H. Gautier,et al.  Fruit load or fruit position alters response to temperature and subsequently cherry tomato quality , 2005 .

[78]  W. Dunn,et al.  Measuring the metabolome: current analytical technologies. , 2005, The Analyst.

[79]  Yves Gibon,et al.  GMD@CSB.DB: the Golm Metabolome Database , 2005, Bioinform..

[80]  R. D. Hall,et al.  A non-directed approach to the differential analysis of multiple LC–MS-derived metabolic profiles , 2005, Metabolomics.

[81]  W. Dunn,et al.  Evaluation of automated electrospray-TOF mass spectrometryfor metabolic fingerprinting of the plant metabolome , 2005, Metabolomics.

[82]  Alisdair R. Fernie,et al.  Profiling of diurnal patterns of metabolite and transcript abundance in potato (Solanum tuberosum) leaves , 2005, Planta.

[83]  Charles L. Guy,et al.  Exploring the Temperature-Stress Metabolome of Arabidopsis1[w] , 2004, Plant Physiology.

[84]  David M. Rocke,et al.  Design and analysis of experiments with high throughput biological assay data. , 2004, Seminars in cell & developmental biology.

[85]  Oliver Fiehn,et al.  A prominent role for the CBF cold response pathway in configuring the low-temperature metabolome of Arabidopsis. , 2004, Proceedings of the National Academy of Sciences of the United States of America.

[86]  B. Denoyes-Rothan,et al.  Quantitative metabolic profiling by 1-dimensional 1H-NMR analyses: application to plant genetics and functional genomics. , 2004, Functional plant biology : FPB.

[87]  A. Fernie,et al.  Metabolite profiling: from diagnostics to systems biology , 2004, Nature Reviews Molecular Cell Biology.

[88]  Kazuki Saito,et al.  Potential of metabolomics as a functional genomics tool. , 2004, Trends in plant science.

[89]  L. Willmitzer,et al.  Towards dissecting nutrient metabolism in plants: a systems biology case study on sulphur metabolism. , 2004, Journal of experimental botany.

[90]  M. Hirai,et al.  Integration of transcriptomics and metabolomics for understanding of global responses to nutritional stresses in Arabidopsis thaliana. , 2004, Proceedings of the National Academy of Sciences of the United States of America.

[91]  W. Weckwerth,et al.  Metabolite profiling in plant biology: platforms and destinations , 2004, Genome Biology.

[92]  D. Kell,et al.  Metabolomics by numbers: acquiring and understanding global metabolite data. , 2004, Trends in biotechnology.

[93]  R. Trethewey.  Metabolite profiling as an aid to metabolic engineering in plants. , 2004, Current opinion in plant biology.

[94]  Ludger Wessjohann,et al.  Profiling of Arabidopsis Secondary Metabolites by Capillary Liquid Chromatography Coupled to Electrospray Ionization Quadrupole Time-of-Flight Mass Spectrometry1 , 2004, Plant Physiology.

[95]  F. Ma,et al.  The sun-exposed peel of apple fruit has higher xanthophyll cycle-dependent thermal dissipation and antioxidants of the ascorbate–glutathione pathway than the shaded peel , 2003 .

[96]  J. Salminen.  Effects of Sample Drying and Storage, and Choice of Extraction Solvent and Analysis Method on the Yield of Birch Leaf Hydrolyzable Tannins , 2003, Journal of Chemical Ecology.

[97]  Gloria M. Coruzzi,et al.  Plant Systems Biology , 2003, Plant Physiology.

[98]  W. Fish,et al.  The effects of frozen storage conditions on lycopene stability in watermelon tissue. , 2003, Journal of agricultural and food chemistry.

[99]  V. Brukhin,et al.  Flower development schedule in tomato Lycopersicon esculentum cv. sweet cherry , 2003, Sexual Plant Reproduction.

[100]  Marianne Defernez,et al.  Factors affecting the robustness of metabolite fingerprinting using 1H NMR spectra. , 2003, Phytochemistry.

[101]  J. Kopka,et al.  Construction and application of a mass spectral and retention time index database generated from plant GC/EI-TOF-MS metabolite profiles. , 2003, Phytochemistry.

[102]  J. Ward,et al.  Assessment of 1H NMR spectroscopy and multivariate analysis as a technique for metabolite fingerprinting of Arabidopsis thaliana. , 2003, Phytochemistry.

[103]  E. de Rijke,et al.  Liquid chromatography with atmospheric pressure chemical ionization and electrospray ionization mass spectrometry of flavonoids with triple-quadrupole and ion-trap instruments. , 2003, Journal of chromatography. A.

[104]  A. Fernie,et al.  Metabolic profiling and biochemical phenotyping of plant systems , 2002, Plant Cell Reports.

[105]  Nigel W. Hardy,et al.  Plant Metabolomics , 2002, The Plant Cell Online.

[106]  Oliver Fiehn,et al.  Analysis of highly polar compounds of plant origin: combination of hydrophilic interaction chromatography and electrospray ion trap mass spectrometry. , 2002, Analytical biochemistry.

[107]  Lloyd W Sumner,et al.  Metabolic profiling of saponins in Medicago sativa and Medicago truncatula using HPLC coupled to an electrospray ion-trap mass spectrometer. , 2002, Phytochemistry.

[108]  U. Roessner,et al.  High-resolution metabolic phenotyping of genetically and environmentally diverse potato tuber systems. Identification of phenocopies. , 2001, Plant physiology.

[109]  J. Görlach,et al.  Growth Stage–Based Phenotypic Analysis of Arabidopsis , 2001, The Plant Cell Online.

[110]  J. Wünsche,et al.  Diurnal changes in non-structural carbohydrates in leaves, phloem exudate and fruit in ‘Braeburn’ apple , 2001 .

[111]  U. Roessner,et al.  Metabolic Profiling Allows Comprehensive Phenotyping of Genetically or Environmentally Modified Plant Systems , 2001, Plant Cell.

[112]  O. Fiehn,et al.  Metabolite profiling for plant functional genomics , 2000, Nature Biotechnology.

[113]  O. Fiehn,et al.  Identification of uncommon plant metabolites based on calculation of elemental compositions using gas chromatography and quadrupole mass spectrometry. , 2000, Analytical chemistry.

[114]  Ute Roessner,et al.  Simultaneous analysis of metabolites in potato tuber by gas chromatography-mass spectrometry. , 2000 .

[115]  R. Bonhomme,et al.  Bases and limits to using 'degree.day' units , 2000 .

[116]  Mark J. Anderson,et al.  DOE Simplified: Practical Tools for Effective Experimentation , 2000 .

[117]  L. Barantin,et al.  Concentration Measurement by Proton NMR Using the ERETIC Method. , 1999, Analytical chemistry.

[118]  R. Trethewey,et al.  Metabolic profiling: a Rosetta Stone for genomics? , 1999, Current opinion in plant biology.

[119]  R. Julkunen‐Tiitto,et al.  Effect of Sample Preparation Method on Birch (Betula pendula Roth) Leaf Phenolics , 1996 .

[120]  B. Markert.  Sample preparation (cleaning, drying, homogenization) for trace element analysis in plant matrices , 1995 .

[121]  G. Wagner,et al.  Basic approaches and methods for quality assurance and quality control in sample collection and storage for environmental monitoring , 1995 .

[122]  Steven A. Hill,et al.  Metabolic control analysis of plant metabolism , 1994 .

[123]  Klaus Hinkelmann,et al.  Design and Analysis of Experiments: Introduction to Experimental Design , 1994 .

[124]  J. Vion-Dury,et al.  Quantitation of metabolites in human blood serum by proton magnetic resonance spectroscopy. A comparative study of the use of formate and TSP as concentration standards , 1992, NMR in biomedicine.

[125]  H. Sauter,et al.  Metabolic profiling of plants: a new diagnostic technique , 1991 .

[126]  R. Julkunen‐Tiitto,et al.  The Effect of the Sample Preparation Method of Extractable Phenolics of Salicaceae Species , 1989, Planta medica.

[127]  I. Rylski,et al.  Effects of floral position and cluster size on fruit development in eggplant , 1983 .

[128]  Royston Goodacre,et al.  Fourier Transform Ion Cyclotron Resonance mass spectrometry for plant metabolite profiling and metabolite identification. , 2012, Methods in molecular biology.

[129]  A. Schaffer,et al.  Precautions for harvest, sampling, storage, and transport of crop plant metabolomics samples. , 2012, Methods in molecular biology.

[130]  Justin J J van der Hooft,et al.  Polyphenol identification based on systematic and robust high-resolution accurate mass spectrometry fragmentation. , 2011, Analytical chemistry.

[131]  Robert D. Hall,et al.  Biology of plant metabolomics , 2011 .

[132]  R. Verpoorte,et al.  Sample preparation for plant metabolomics. , 2010, Phytochemical analysis : PCA.

[133]  Royston Goodacre,et al.  An Introduction to Liquid Chromatography– Mass Spectrometry Instrumentation Applied in Plant Metabolomic Analyses † Untargeted Plant Metabolomics and the Potential of Liquid Chromatography Mass Spectrometry , 2022 .

[134]  Mark R Viant,et al.  Two-dimensional J-resolved NMR spectroscopy: review of a key methodology in the metabolomics toolbox. , 2010, Phytochemical analysis : PCA.

[135]  J. Schripsema,et al.  Application of NMR in plant metabolomics: techniques, problems and prospects. , 2010, Phytochemical analysis : PCA.

[136]  A. Fernie,et al.  Metabolomics-assisted breeding: a viable option for crop improvement? , 2009, Trends in genetics : TIG.

[137]  T. Mexia,et al.  Author ' s personal copy , 2009 .

[138]  Joachim Kopka,et al.  Nonsupervised construction and application of mass spectral and retention time index libraries from time-of-flight gas chromatography-mass spectrometry metabolite profiles. , 2007, Methods in molecular biology.

[139]  Alfred Ross,et al.  Chapter 3 – NMR Spectroscopy Techniques for Application to Metabonomics , 2007 .

[140]  Wolfram Weckwerth,et al.  Metabolomics : methods and protocols , 2007 .

[141]  Y. Ba,et al.  Proton NMR determination of Mg2+ and Ca2+concentrations using tetrasodium EDTA complexes , 2007 .

[142]  John C. Lindon,et al.  The handbook of metabonomics and metabolomics , 2007 .

[143]  R. Hall,et al.  Plant metabolomics: from holistic hope, to hype, to hot topic. , 2006, The New phytologist.

[144]  Robert D. Hall,et al.  Plant metabolomics strategies based upon quadrupole time of flight mass spectrometry (QTOF-MS) , 2006 .

[145]  Johan Trygg,et al.  Chemometrics in Metabolomics — An Introduction , 2006 .

[146]  Jane L. Ward,et al.  NMR Spectroscopy in Plant Metabolomics , 2006 .

[147]  J. Kopka.  Gas chromatography mass spectrometry , 2006 .

[148]  Lloyd W. Sumner,et al.  Current Status and Forward Looking Thoughts on LC/MS Metabolomics , 2006 .

[149]  Robert D. Hall,et al.  Breakthrough Technologies A Novel Approach for Nontargeted Data Analysis for Metabolomics . Large-Scale Profiling of Tomato Fruit Volatiles 1 [ w ] , 2005 .

[150]  A. Fernie,et al.  Metabolic profiling of leaves and fruit of wild species tomato: a survey of the Solanum lycopersicum complex. , 2005, Journal of experimental botany.

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

[152]  R. Goodacre,et al.  Metabolic Profiling: Its Role in Biomarker Discovery and Gene Function Analysis , 2003, Springer US.

[153]  O. Fiehn,et al.  Research erratum , 2001, Nature Biotechnology.

[154]  T. Fan.  Metabolite profiling by one- and two-dimensional NMR analysis of complex mixtures , 1996 .

[155]  O. Kempthorne,et al.  Introduction to experimental design , 1994 .

[156]  Catherine Douillard,et al.  The aroma of strawberry (Fragaria ananassa): characterisation of some cultivars and influence of freezing. , 1990 .