Metabolic fingerprinting reveals a novel candidate biomarker for prednisolone treatment in cattle

详细信息    查看全文

• 作者：Nathalie De Clercq ; Julie Vanden Bussche ; Lieven Van Meulebroek…
• 关键词：Metabolomics ; Prednisolone ; Biomarker ; Bovine urine ; In vivo ; UHPLC ; HRMS
• 刊名：Metabolomics
• 出版年：2016
• 出版时间：January 2016
• 年：2016
• 卷：12
• 期：1
• 全文大小：1,102 KB
• 参考文献：Adams, J. E., Bodor, G. S., Dávila-Román, V. G., et al. (1993). Cardiac troponin I. A marker with high specificity for cardiac injury. Circulation, 88(1), 101–106.PubMed CrossRef
  Arioli, F., Fidani, M., Casati, A., Fracchiolla, M. L., & Pompa, G. (2010). Investigation on possible transformations of cortisol, cortisone and cortisol glucuronide in bovine faecal matter using liquid chromatography-mass spectrometry. Steroids, 75(4), 350–354.PubMed CrossRef
  Behrens, T., Bonberg, N., Casjens, S., Pesch, B., & Brüning, T. (2014). A practical guide to epidemiological practice and standards in the identification and validation of diagnostic markers using a bladder cancer example. Biochimica et Biophysica Acta, 1844, 145–155.PubMed CrossRef
  Bertocchi, L., Dusi, G., Ghidelli, V., et al. (2013). Investigation on the origin of prednisolone in urine and adrenal glands of cows. Food Additives & Contaminants. Part A, Chemistry, Analysis, Control, Exposure & Risk Assessment, 30(6), 1055–1062.CrossRef
  Blokland, M. H., Van Tricht, E. F., Van Rossum, H. J., Sterk, S. S., & Nielen, M. W. F. (2012). Endogenous steroid profiling by gas chromatography-tandem mass spectrometry and multivariate statistics for the detection of natural hormone abuse in cattle. Food Additives and Contaminants. Part A, Chemistry, Analysis, Control, Exposure and Risk Assessment, 29(7), 1030–1045.PubMed
  Buisson, C., Hebestreit, M., Weigert, A. P., et al. (2005). Application of stable carbon isotope analysis to the detection of 17beta-estradiol administration to cattle. Journal of Chromatography A, 1093(1–2), 69–80.PubMed CrossRef
  Bulska, E., Gorczyca, D., Zalewska, I., Pokrywka, A., & Kwiatkowska, D. (2014). Analytical approach for the determination of steroid profile of humans by gas chromatography isotope ratio mass spectrometry aimed at distinguishing between endogenous en exogenous steroids. Journal of Pharmaceutical and Biomedical Analysis,. doi:10.​1016/​j.​jpba.​2014.​11.​017 .PubMed
  Cannizzo, F. T., Capra, P., Divari, S., Ciccotelli, V., Biolatti, B., & Vincenti, M. (2011). Effects of low-dose dexamethasone and prednisolone long term administration in beef calf: Chemical and morphological investigation. Analytica Chimica Acta, 700, 95–104.PubMed CrossRef
  Chau, C. H., Rixe, O., McLeod, H., & Figg, W. D. (2008). Validation of analytical methods for biomarkers employed in drug development. Clinical Cancer Research, 14(19), 5967–5976.PubMed PubMedCentral CrossRef
  Churchwell, M. I., Twaddle, N. C., Meeker, L. R., & Doerge, (2005). Improving LC-MS sensitivity through increases in chromatographic performance: comparisons of UPLC-ES/MS/MS to HPLC-ES/MS/MS. Journal of Chromatography B. Analytical Technologies in the Biomedical and Life Sciences, 825(2), 134–143.PubMed CrossRef
  Commission Decision 2002/657/EC (2002). Official Journal of the European Community L221:8. Retrieved February 12, 2015 from http://​eur-lex.​europa.​eu/​LexUriServ/​LexUriServ.​do?​uri=​OJ:​L:​2002:​221:​0008:​0036:​EN:​PDF .
  Commission Decision 96/23/EC (1996). Official Journal of the European Community, L125, 10-32. Retrieved February 12, 2015 from http://​eur-lex.​europa.​eu/​legal-content/​NL/​TXT/​PDF/​?​uri=​CELEX:​31996L0023&​from=​EN .
  Commission Regulation 37/2010 (2010). Official Journal of the European Community, No. L15/1, 11, 26, 47 and 56. Retrieved February 12, 2015 from http://​ec.​europa.​eu/​health/​files/​eudralex/​vol-5/​reg_​2010_​37/​reg_​2010_​37_​en.​pdf .
  Commission staff working document on the implementation of national residue monitoring plans in the member states in 2009 (2009). Brussel, Belgium. Retrieved February 12, 2015 from http://​ec.​europa.​eu/​food/​food/​chemicalsafety/​residues/​workdoc_​2009_​en.​pdf .
  Commission staff working document on the implementation of national residue monitoring plans in the member states in 2010, Brussel, Belgium. . Retrieved February 12, 2015 from http://​ec.​europa.​eu/​food/​food/​chemicalsafety/​residues/​workdoc_​2010_​en.​pdf .
  Commission staff working document on the implementation of national residue monitoring plans in the member states in 2011, Brussel, Belgium. . Retrieved February 12, 2015 from http://​ec.​europa.​eu/​food/​food/​chemicalsafety/​residues/​docs/​workdoc_​2011_​en.​pdf .
  Commission staff working document on the implementation of national residue monitoring plans in the member states in 2012, Brussel, Belgium. . Retrieved February 12, 2015 from http://​ec.​europa.​eu/​food/​food/​chemicalsafety/​residues/​docs/​workdoc_​2012_​en.​pdf .
  De Clercq, N., Vanden Bussche, J., Croubels, S., Delahaut, P., & Vanhaecke, L. (2013). A validated analytical method to study the long-term stability of natural and synthetic glucocorticoids in livestock urine using ultra-high performance liquid chromatography coupled to Orbitra-high resolution mass spectrometry. Journal of Chromatography A, 1301, 111–121.PubMed CrossRef
  de la Torre, X., González, J. C., Pichini, S., Pascual, J. A., & Segura, J. (2001). 13C/12C isotope ratio MS analysis of testosterone, in chemicals and pharmaceutical preparations. Journal of Pharmaceutical and Biomedical Analysis, 24(4), 645–650.PubMed CrossRef
  de Rijke, E., Zoontjes, P. W., Samson, D., Oostra, S., Sterk, S. S., & van Ginkel, L. A. (2014). Investigation of the presence of prednisolone in bovine urine. Food Additives and Contaminants. Part A, Chemistry, Analysis, Control, Exposure and Risk Assessments, 31(4), 605–613.
  Díaz, R., Pozo, O. J., Sancho, J. V., & Hernández, F. (2014). Metabolomic approaches for orange origin discrimination by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry. Food Chemistry, 157, 84–93.PubMed CrossRef
  Dietmair, S., Hodson, M. P., Quek, L. E., Timmins, N. E., Gray, P., & Nielsen, L. K. (2012). A multi-omics analysis of recombinant protein production in Hek293 cells. PLoS One, 7(8), 1–15.CrossRef
  Eriksson, L., Trygg, J., & Wold, S. (2007). CV-ANOVA for significance testing of PLS and OPLS® models. Journal of Chemometrics, 22(11–12), 594–600.
  EURL (European Union Reference Laboratory). (2014). EURL Reflection paper: Natural growth promoting substances in biological samples. Presence—and formation—of hormones and other growth promoting substances in food producing animals. Current approaches for enforcement and research needs for full implementation in residue control. Rikilt Wageningen UR.
  Ferranti, C., delli Quadri, F., Palleschi, L., et al. (2011). Studies on the presence of natural and synthetic corticosteroids in bovine urine. Steroids, 76(6), 616–625.PubMed CrossRef
  Ferranti, C., Famele, M., Palleschi, L., Bozzetta, E., Pezzolato, M., & Draisci, R. (2013). Excretion profile of corticosteroids in bovine urine compared with tissue residues after therapeutic and growth-promoting administration of dexamethasone. Steroids, 78(9), 803–812.PubMed CrossRef
  Gika, H. G., Theodoridis, G. A., Plumb, R. S., & Wilson, I. D. (2014). Current practice of liquid chromatography–mass spectrometry in metabolomics and metabonomics. Journal of Pharmaceutical and Biomedical Analysis, 87, 12–25.PubMed CrossRef
  Goniewicz, M. L., Havel, C. M., Peng, M. W., et al. (2009). Elimination kinetics of the tobacco-specific biomarker and lung carcinogen 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol. Cancer Epidemiology, Biomarker and Prevention, 18(12), 3421–3425.CrossRef
  Grund, B., & Sabin, C. (2010). Analysis of biomarker data: logs, odds ratio and ROC curves. Current Opinion in HIV and AIDS, 5(6), 473–479.PubMed PubMedCentral CrossRef
  Hardy, R. S., Raza, K., & Cooper, M. S. (2012). Endogenous glucocorticoids in inflammation: Contributions of systemic and local responses. Swiss Medical Weekly, 142, 1–10.
  Hawkins, D. M., Basak, S. C., & Mills, D. (2003). Assessing model fit by cross-validation. Journal of Chemical Information and Modeling, 43(2), 579–586.CrossRef
  Hjerpsted, J. B., Ritz, C., Schou, S. S., Tholstrup, T., & Dragsted, L. O. (2014). Effect of cheese and butter intake on metabolites in urine using an untargeted metabolomics approach. Metabolomics, 10(6), 1176–1185.CrossRef
  Hunter, D. J., Losina, E., Guermazi, A., Burstein, D., Lassere, M. N., & Kraus, V. (2010). A pathway and approach to biomarker validations and quantification of osteoarthritis clinical trails. Current Drug Targets, 11(5), 536–545.PubMed PubMedCentral CrossRef
  Jacob, C. C., Pinel, G., Biancotto, G., & Le Bizec, B. (2014). Evaluation of specific gravity as normalization strategy for cattle urinary metabolome analysis. Metabolomics, 10, 627–637.CrossRef
  Jia, W., Ling, Y., Lin, Y. H., Chang, J., & Chu, X. (2014). Analysis of additives in diary products by liquid chromatography coupled to quadrupole-orbitrap mass spectrometry. Journal of Chromatography A, 1336, 67–75.PubMed CrossRef
  Jung, Y. J., Lee, H. S., Kang, D. G., et al. (2011). 1H-NMR-based metabolomics study of cerebral infarction. Stroke, 42(5), 1282–1288.PubMed CrossRef
  Kaabia, Z., Pinel, G., Popot, M. A., Chouribery, L., Plou, P., Bonnaire, Y., & Le Bizec, B. (2013). Monitoring the endogenous steroid profile disruption in urine and blood upon nandrolone administration: An efficient and innovative strategy to screen for nandrolone abuse in entire male horses. Drug Testing and Analysis, 6, 376–388.PubMed CrossRef
  Koulman, A., Lane, G. A., Harrison, S. J., & Volmer, D. A. (2009). From differentiating metabolites to biomarkers. Analytical and Bioanalytical Chemistry, 394(4), 663–670.PubMed PubMedCentral CrossRef
  Lee, J. W., Devanarayan, V., Barrett, Y. C., et al. (2006). Fit-for-purpose method development and validation for successful biomarker measurement. Pharmaceutical Research, 23(2), 312–328.PubMed CrossRef
  Leporati, M., Capra, P., Cannizzo, F. T., Biolatti, B., Nebbia, C., & Vincenti, M. (2013). Determination of prednisolone metabolites in beef cattle. Food Additives and Contaminants. Part A, Chemistry, Analysis, Control, Exposure and Risk Assessment, 30(6), 1044–1054.PubMed
  Levine, L., & Fahy, J. P. (1945). Evaluation of urinary lead determinations. The Journal of Industrial Hygiene and Toxicology, 27, 217–223.
  Marshall, A. G. (2000). Milestones in Fourier transform ion cyclotron resonance mass spectrometry technique development. International Journal of Mass Spectrometry and Ion Processes, 200(1–3), 331–356.CrossRef
  Matabosch, X., Pozo, O. J., Monfort, N., et al. (2013). Urinary profile of methylprednisolone and its metabolites after oral and topical administrations. The Journal of Steroid Biochemistry and Molecular Biology, 138, 214–221.PubMed CrossRef
  Matsui, S. (2006). Reducing false positive findings in statistical analysis of pharmacogenomics biomarker studies using high-throughput technologies. Current Drug Safety, 1(2), 135–141.PubMed CrossRef
  Matthew, B., & William, R. (2003). Partial least squares for discrimination. Journal of Chemometrics, 17(3), 166–173.CrossRef
  McLoughlin, N., Yin, D., Maltby, L., Wood, R. M., & Yu, H. (2000). Evaluation of sensitivity and specificity of two crustacean biochemical biomarkers. Environmental Toxicology and Chemistry, 19(8), 2085–2092.CrossRef
  Neumann, S., & Böcker, S. (2010). Computational mass spectrometry for metabolomics: Identification of metabolites and small molecules. Analytical and Bioanalytical Chemistry, 398(7–8), 2779–2788.PubMed CrossRef
  Parikh, C. R., & Philbrook, H. T. (2014). Key concepts and limitations of statistical methods for evaluating biomarkers of kidney disease. Journal of the American Society of Nephrology, 25(8), 1621–1629.PubMed PubMedCentral CrossRef
  Pepe, M. S., Janes, H., Longton, G., Leisenring, W., & Newcomb, P. (2004). Limitations of the odds ratio in gauging the performance of a diagnostic prognostic, or screening marker. American Journal of Epidemiology, 159(9), 882–890.PubMed CrossRef
  Pinel, G., Chereau, S., Cesbron, N., Monteau, F., & Le Bizec, B. (2015). LC-HRMS based metabolomics screening model to detect various β-agonists treatments in bovines. Metabolomics, 11, 403–411.CrossRef
  Pinel, G., Rambaud, L., Monteau, F., Elliot, C., & Le Bizec, B. (2010). Estranediols profiling in calves’ urine after 17β-nandrolone laureate ester administration. The Journal of Steroid Biochemistry and Molecular Biology, 121(3–5), 626–632.PubMed CrossRef
  Pinel, G., Weigel, S., Lommen, A., et al. (2011). Assessment of two complementary liquid chromatography coupled to high resolution mass spectrometry metabolomics strategies for the screening of anabolic steroid treatments in calves. Analytica Chimica Acta, 700(1–2), 144–154.CrossRef
  Pompa, G., Arioli, F., Casati, A., Fidani, M., Bertocchi, L., & Dusi, G. (2011). Investigation of the origin of prednisolone in cow urine. Steroids, 76(1–2), 104–110.PubMed CrossRef
  Puntmann, V. O. (2009). How-to guide on biomarkers: Biomarker definitions, validation and applications with examples from cardiovascular disease. Postgraduate Medical Journal, 85(1008), 538–545.PubMed CrossRef
  Quintás, G., Portillo, N., García-Cañaveras, J. C., Castell, J. V., Ferrer, A., & Lahoz, A. (2012). Chemometric approaches to improve PLSDA model outcome for predicting human non-alcoholic fatty liver disease using UHPLC-MS as a metabolomic profiling tool. Metabolomics, 8(1), 86–98.CrossRef
  Regal, P., Seijas, A., Cepeda, A., & Fente, C. (2013). Structure elucidation and HPLC-MS/MS determination of a potential biomarker for estradiol administration in cattle. Analytical and Bioanalytical Chemistry, 405(29), 9537–9546.PubMed CrossRef
  Scalbert, A., Brennan, L., Fiehn, O., et al. (2009). Mass-spectrometry-based metabolomics: Limitations and recommendations for future progress with particular focus on nutrition research. Metabolomics, 5(4), 435–458.PubMed PubMedCentral CrossRef
  Scarth, J., Clarcke, A., Hands, J., Tealt, P., Macarthur, R., & Kay, J. (2010). Validation of a quantitative multi-residue urinary assay for the detection of androgen, oestrogen and progestagen abuse in the bovine. Chromatographia, 71(3), 241–252.CrossRef
  Shah, V. P., Midha, K. K., & Findlay, J. W. A. (2000). Bioanalytical method validation-a revisit with a decade of progress. Pharmaceutical Research, 17(12), 1551–1557.PubMed CrossRef
  Snyder, L. R., Kirkland, J. J., & Glajch, J. L. (1997). Practical HPLC method development (2nd ed.). London: Wiley.CrossRef
  Soininen, T. H., Jukarainen, N., Auriola, S. O. K., Julkunen-Tiitto, R., Karjalainen, R., & Vepsäläinen, J. J. (2014). Quantitative metabolite profiling of edible onion species by NMR and HPLC-MS. Food Chemistry, 165, 499–505.PubMed CrossRef
  Sumner, L. W., Amberg, A., Barrett, D., et al. (2007). Proposed minimum reporting standards for chemical analysis Chemical Analysis Working Group (CAWG) Metabolomics Standards Initiative (MSI). Metabolomics, 3(3), 211–221.PubMed PubMedCentral CrossRef
  Tardieu, A., De Man, W., & This, H. (2010). Using one-dimensional (1D) and two-dimensional (2D) quantitative proton (1H) nuclear magnetic resonance spectroscopy (q NMR) for the identification and quantification of taste compounds in raw onion (Allium cepa L.) bulbs and in aqueous solutions where onion tissues are soaked. Analytical and Bioanalytical Chemistry, 398(7–8), 3139–3153.PubMed CrossRef
  Theodoridis, G. A., Gika, H. G., Want, E. J., & Wilson, I. D. (2012). Liquid chromatography-mass spectrometry based global metabolite profiling: A review. Analytica Chimica Acta, 711, 7–16.PubMed CrossRef
  Trygg, J., & Wold, S. (2002). Orthogonal projections to latent structures (O-PLS). Journal of Chemometrics, 16(3), 119–128.CrossRef
  van den Berg, R. A., Hoefsloot, H. C. J., Westerhuis, J. A., Smilde, A. K., & van der Werf, M. J. (2006). Centering, scaling, and transformations: improving the biological information content of metabolomics data. BMC Genomics, 7, 142–156.PubMed PubMedCentral CrossRef
  Van Meulebroek, L., Vanden Bussche, J., De Clercq, N., Steppe, K., & Vanhaecke, L. (2014). A metabolomics approach to unravel the regulating role of phytohormones towards carotenoid metabolism in tomato fruit. Metabolomics,. doi:10.​1007/​s1130601407289 .
  Verhagen, H., Coolen, S., Duchateau, G., Hamer, M., Kyle, J., & Rechner, A. (2004). Assessment of the efficacy of functional food ingredients—introducing the concept “kinetics of biomarkers”. Mutation Research, 551(1–2), 65–78.PubMed CrossRef
  Vincenti, M., Girolami, F., Capra, P., et al. (2009). Study of dexamethasone urinary excretion profile in cattle by LC-MS/MS: Comparison between therapeutic and growth-promoting administration. Journal of Agricultural and Food Chemistry, 57(4), 1299–1306.PubMed CrossRef
  Vincenti, M., Leporati, M., Capra, P., et al. (2012). A field survey on the presence of prednisolone and prednisone in urine samples from untreated cows. Food Additives and Contaminants. Part A, Chemistry, Analysis, Control, Exposure and Risk Assessment, 29(12), 1893–1900.PubMed
  Wagner, J. A. (2002). Overview of biomarkers and surrogate endpoints in drug development. Disease Markers, 18(2), 41–46.PubMed PubMedCentral CrossRef
  Weiss, S. H., Goedert, J. J., Sarngadharan, M. G., Bodner, A. J., Gallo, R. C., & Blattner, W. A. (1985). Screening test for HTLV-III (AIDS agent) antibodies. Specificity, sensitivity and applications. JAMA, 253(2), 221–225.PubMed CrossRef
  Wetenschappelijk Comité van het Federaal Agentschap voor de veiligheid van de voedselketen, (2013). Retrieved February 12, 2015 from http://​www.​afsca.​be/​wetenschappelijk​comite/​adviezen/​_​documents/​ADVIES07-2013_​NL_​DossierSciCom201​2-07.​pdf .
  Wicklund, S., Johansson, E., Sjöström, L., et al. (2008). Visualization of GC/TOF-MS-based metabolomics data for identification of biochemically interesting compounds using OPLS class models. Analytical Chemistry, 80(1), 115–122.CrossRef
  Wold, S., Sjöström, M., & Eriksson, L. (2001). PLS-regression: A basic tool of chemometrics. Chemometrics and Intelligent Laboratory Systems, 58(2), 109–130.CrossRef
  Wolf, S., Schmidt, S., Müller-Hannemann, M., & Neumann, S. (2010). In silico fragmentation for computer assisted identification of metabolite mass spectra. BMC Bioinformatics, 11, 148–160.PubMed PubMedCentral CrossRef
  Xue, S. Y., Li, Z. Y., Zhi, H. J., et al. (2012). Metabolic fingerprinting investigation of Tussilago farfara L. by GC-MS and multivariate data analysis. Biochemical Systematics and Ecology, 41, 6–12.CrossRef
  
• 作者单位：Nathalie De Clercq (1)
  Julie Vanden Bussche (1)
  Lieven Van Meulebroek (1)
  Siska Croubels (2)
  Philippe Delahaut (3)
  Dieter Buyst (4)
  José Martins (4)
  Jianru Stahl-Zeng (5)
  Lynn Vanhaecke (1)
  
  1. Laboratory of Chemical Analysis, Department of Veterinary Public Health & Food Safety, Faculty of Veterinary Medicine, Ghent University, Salisburylaan 133, 9820, Merelbeke, Belgium
  2. Laboratory of Pharmacology and Toxicology, Department of Pharmacology, Toxicology and Biochemistry, Faculty of Veterinary Medicine, Ghent University, Salisburylaan 133, 9820, Merelbeke, Belgium
  3. Département Santé, CER Groupe, Rue du Point du Jour 8, 6900, Marloie, Belgium
  4. NMR and Structural Analysis Research Unit, Department of Organic and Macromolecular Chemistry, Faculty of Sciences, Ghent University, Krijgslaan 281 S4, 9000, Ghent, Belgium
  5. SCIEX, Landwehrstrasse 54, 64293, Darmstadt, Germany
  
• 刊物主题：Biochemistry, general; Molecular Medicine; Cell Biology; Developmental Biology; Biomedicine general;
• 出版者：Springer US
• ISSN：1573-3890

文摘

The use of glucocorticoids as growth promoters for meat-producing animals is strictly regulated within the European Union. However, in the past few years, a higher frequency of non-compliant bovine urine samples for prednisolone has been noticed, which could not be directly related to fraudulent use of prednisolone. As such, questions have risen about the origin of this compound. Unfortunately, at present, no decisive strategy has been established to discriminate between endogenous and exogenous prednisolone. In this study, an untargeted metabolomics strategy, based on Orbitrap and QqTOF mass spectrometry, was deployed to reveal urinary biomarkers, which are indicative for the exogenous administration of the synthetic glucocorticoid prednisolone. For this purpose, prednisolone was administered intramuscularly and per os to 12 bovines and a total of 2700 urine samples were collected before, during and after treatment. Multivariate statistical data analysis (i.e. OPLS-DA) revealed four differentiating metabolites that allowed discrimination between urine samples collected before and during prednisolone administration. None of these compounds were present in urine containing endogenous prednisolone, of which the formation was induced by the administration of a synthetic analogue of adrenocorticotropic hormone. Only one metabolite was retained as a highly suitable biomarker during growth-promoting and therapeutic prednisolone treatment, with 93.4 % sensitivity and 96.3 % specificity. Besides, this compound could be detected up to 4 days after a single therapeutic per os prednisolone administration. Based on accurate mass, isotope pattern, and MS/MS spectra, this compound was putatively annotated and is suggested as an actionable biomarker for exogenous prednisolone administration.