Methods in Enzymology. Volume XXXVIII. Hormone Action. Part C Cyclic Nucleotides. Joel G. Hardman. Bert W. O'Malley

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1 Methods in Enzymology Volume XXXVIII Hormone Action Part C Cyclic Nucleotides Joel G. Hardman Bert W. O'Malley

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3 CONTRIBUTORS TO VOLUME XXXVIII PREFACE VOLUMES IN SERIES x xiv xvi EARL W. SUTHERLAND, JR. ( ) xxi Section I. Extraction and Purification of Cyclic Nucleotide s 1. Rapid Tissue Fixation and Extraction STEVEN E. MAYER, Techniques JAMES T. STULL, AN D WILLIAM B. WASTILA 3 2. Separation and Purification of Cyclic Nucleo - tides by Ion-Exchange Resin Column G. SCHULTZ, E. BöHME, Chromatography AND J. G. HARDMAN 9 3. Separation, Purification, and Analysis of Cyclic Nucleotides by High Pressure Ion-Exchang e Chromatography GARY BROOKER Separation of Cyclic Nucleotides by Thin- Layer Chromatography on Polyethyleneimine E. BÖHME AND G. SCHULT Z Cellulose Isolation of Cyclic AMP by Inorganic Salt PETER S. CHAN AN D Coprecipitation MICHAEL C. LIN Separation and Purification of Cyclic Nucleo - tides by Alumina Column Chromatography ARNOLD A. WHITE 41 Section II. Assay of Cyclic Nucleotides 7. Assay of Cyclic Nucleotides by Receptor Pro- ALFRED G. GILMAN AN D tein Binding Displacement FERID MURAD Assay of Cyclic AMP by the Luciferin- CHARLES A. SUTHERLAND Luciferase System AND R. A. JOHNSON Assay of Cyclic AMP by Protein Kinase STEVEN E. MAYER, Activation JAMES T. STULL, WILLIAM B. WASTILA, AN D BARBARA THOMPSON Quantitation of Cyclic GMP by Enzymatic NELSON D. GOLDBERG AND Cycling MARI K. HADDOX 73

4 11. The Measurement of Cyclic GMP with ROBERT F. O'DE A Escherichia coli Elongation Factor Tu JAMES W. BODLEY, LILLIAN LIN, MARI K. HADDOX, AND NELSON D. GOLDBERG Assay of Cyclic GMP by Activation of Cyclic J. F. Kuo AND GMP-Dependent Protein Kinase PAUL GREENGARD Assay of Cyclic Nucleotides by Radioimmuno - assay Methods ALTON L. STEINER Determination of Cyclic GMP by Formation GUNTER SCHULTZ AN D of [ß-'ZP]GDP JOEL G. HARDMAN 10 6 Section III. Biosynthesis of Cyclic Nucleotides 15. General Principles of Assays for Adenylat e Cyclase and Guanylate Cyclase Activity GÜNTER SCHULTZ An Automated Chromatographic Assay fo r Adenylate Cyclase and Cyclic 3', 5'-AMP Phosphodiesterase MICHAEL C. LIN Preparation of Particulate and Detergent-Dis- ROGER A. JOHNSON AND persed Adenylate Cyclase from Brain EARL W. SUTHERLAND Preparation and Characterization of Adenylate GEORGE I. DRUMMOND AND Cyclase from Heart and Skeletal Muscle DAVID L. SEVERSON Adenylate Cyclase from Kidney and Bone S. J. MARX AND G. D. AURBACH Preparation of Vertebrate Photoreceptor Membranes for Study of Adenylate Cyclase, Guanylate Cyclase, and Cyclic Nucleotide J. J. KEIRNS, N. MIKI, Phosphodiesterase AND M. W. BITENSKY Preparation and Properties of Adenylate Cyclase from Escherichia coli MARIANO TAO 15 5 KATSUJI TAKAI, 22. Adenylate Cyclase from Brevibacterium YOSHIKAZU KURASHINA, liquefaciens AND OSAMU HAYAISHI Preparation of Adenylate Cyclase from Frog JACK ERLICHMAN AN D Erythrocytes ORA M. ROSEN Method for Solubilization of Myocardial Adenylate Cyclase and Assessment of th e Role of Phospholipids in Hormon e Stimulation GERALD S. LEVEY Production of Glass Bead-Immobilized J. CRAIG VENTER AN D Catecholamines JACK E. DixoN 180

5 26. A Partial Purification of the ß-Adrenergi c Receptor Adenylate Cyclase Complex b y Affinity Chromatography to Glass Bead- J. CRAIG VENTER AN D Immobilized Isoproterenol NATHAN O. KAPLAN Preparation and Characterization of Guanylate ARNOLD A. WHITE AND Cyclase from Bovine Lung TERRY V. ZENSER Guanylate Cyclase from Sperm of the Sea DAVID L. GABBERS AND Urchin, Strongylocentrotus purpuratus J. P. GRAY Guanylate Cyclase in Human Platelets EYCKE BÖHME, REGINE JUNG, AND ILSE MECHLER 19 9 Section IV. Degradation of Cyclic Nucleotide s 30. Assay of Cyclic Nucleotide Phosphodiesterases W. JOSEPH THOMPSON, with Radioactive Substrates GARY BROOKER, AND M. MICHAEL APPLEMAN Assay of Cyclic Nucleotide Phosphodiesterase by a Continuous Titrimetric Technique WAI YIU CHEUNG Cyclic 3',5'-Nucleotide Phosphodiesterase fro m Bovine Heart R. W. BUTCHER Purification and Characterization of Cycli c 3',5'-Nucleotide Phosphodiesterase from WAI YIU CHEUNG AND Bovine Brain YING MING LIN Purification and Characterization of Cyclic Nucleotide Phosphodiesterase from Skeletal ROBERT G. KEMP AN D Muscle YUNG-CHEN HUANG Purification and Properties of Cyclic Nucleo - tide Phosphodiesterase from Dictyostelium BRUCE M. CHASSY AND discoideum (Extracellular) E. VICTORIA PORTER Cyclic AMP Phosphodiesterase of Escherichia LARRY D. NIELSEN AND soli H. V. RICKENBERG Preparation and Characterization of Multiple WESLEY L. TERASAKI, Forms of Cyclic Nucleotide Phosphodiester- THOMAS R. RussELL, AND ase from Liver M. MICHAEL APPLEMAN Activity Stain for the Detection of Cyclic ELIHU N. GOREN, Nucleotide Phosphodiesterase in Polyacryla- ALLEN H. HIRSCH, AN D mide Gels ORA M. ROSEN Purification and Characterization of a Protein YING MING LIN, Activator of Cyclic Nucleotide Phospho- YUNG PIN LIU, AN D diesterase from Bovine Brain WAI YIU CHEUNG 262

6 40. Techniques for the Formation, Partial Purification, and Assay of a Cyclic AMP Inhibitor FERID MURAD 273 Section V. Cyclic Nucleotide-Dependent Protein Kinases an d Binding Proteins 41. Assay of Cyclic AMP-Dependent Protein JACKIE D. CORBIN AN D Kinases ERWIN M. REIMANN Criteria for the Classification of Protein J. A. TRAUGH, Kinases C. D. ASHBY, AN D D. A. WALSH Preparation of Homogeneous Cyclic AMP- J. A. BEAVO, Dependent Protein Kinase(s) and Its Sub- P. J. BECHTEL, AND units from Rabbit Skeletal Muscle E. G. KREBS Cyclic AMP-Dependent Protein Kinase from CHARLES S. RUBIN, Bovine Heart Muscle JACK ERLICHMAN, AN D ORA M. ROSEN Preparation and Properties of Cyclic AMP - Dependent Protein Kinases from Rabbit Red Blood Cells MARIANO TAO Cytoplasmic Hepatic Protein Kinases LEE-JING CHEN AND DONAL A. WALSH Purification and Characterization of Cyclic J. F. Kuo AN D GMP-Dependent Protein Kinases PAUL GREENGARD Purification and Characterization of an Inhibitor Protein of Cyclic AMP-Dependent Pro- C. DENNIS ASHBY AN D tein Kinases DONAL A. WALSH Techniques for the Study of Protein Kinase THOMAS R. SODERLING, Activation in Intact Cells JACKIE D. CORBIN, AN D CHARLES R. PARK The Purification and Analysis of Mechanism IRA PASTAN, of Action of a Cyclic AMP-Receptor Pro- MARIA GALLO, AN D tein from Escherichia colt WAYNE B. ANDERSON The Detection and Characterization of Cyclic GORDON N. GILL AND AMP-Receptor Proteins in Animal Cells GORDON M. WALTON 37 6 Section VI. Synthetic Derivatives of Cyclic Nucleotides and Their Precursors 52. The Preparation and Use of Cyclic AMP MEIR WILCHEK AND Sepharose ZVI SELINGER The Preparation and Use of Diazomalonyl Derivatives in Isolating and Identifying BARRY S. COOPERMAN AND Cyclic AMP Receptor Sites DAVID J. BRUNSWICK 387

7 54. The Preparation of Acylated Derivatives of T. POSTERNAK AN D Cyclic Nucleotides G. WEIMANN The Synthesis of ["P] Adenosine 3',5'-Cyclic Phosphate and Other Ribo- and Deoxyribonucleoside 3',5'-Cyclic Phosphates R. H. SYMONS Adenylylimidodiphosphate and Guanylylimi - dodiphosphate RALPH G. YOUNT The Synthesis of 1,N6-Ethenoadenosine 3',5' - Monophosphate ; A Fluorescent Analog of Cyclic AMP JOHN A. SECRIST III 428 AUTHOR INDEX 43 1 SUBJECT INDEX 440