Biochemistry 2/e - Garrett & Grisham CHAPTER 5 Proteins: Their Biological Functions and Primary Structure to accompany Biochemistry, 2/e by Reginald Garrett and Charles Grisham All rights reserved. Requests for permission to make copies of any part of the work should be mailed to: Permissions Department, Harcourt Brace & Company, 6277 Sea Harbor Drive, Orlando, Florida 32887-6777 Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Outline • • • • • • 5.1 Proteins - Linear Polymers of Amino Acids 5.2 Architecture 5.3 Many Biological Functions 5.4 May be Conjugated with Other Groups 5.7 Primary Structure Determination 5.8 Consider the Nature of Sequences Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham 5.1 Proteins are Linear Polymers of Amino Acids Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham The Peptide Bond • is usually found in the trans conformation • has partial (40%) double bond character • is about 0.133 nm long - shorter than a typical single bond but longer than a double bond • Due to the double bond character, the six atoms of the peptide bond group are always planar! • N partially positive; O partially negative Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham The Coplanar Nature of the Peptide Bond Six atoms of the peptide group lie in a plane! Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham “Peptides” • • • • • • Short polymers of amino acids Each unit is called a residue 2 residues - dipeptide 3 residues - tripeptide 12-20 residues - oligopeptide many - polypeptide Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham “Protein” One or more polypeptide chains • One polypeptide chain - a monomeric protein • • • • • More than one - multimeric protein Homomultimer - one kind of chain Heteromultimer - two or more different chains Hemoglobin, for example, is a heterotetramer It has two alpha chains and two beta chains Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Proteins - Large and Small • Insulin - A chain of 21 residues, B chain of 30 residues -total mol. wt. of 5,733 • Glutamine synthetase - 12 subunits of 468 residues each - total mol. wt. of 600,000 • Connectin proteins - alpha - MW 2.8 million! • beta connectin - MW of 2.1 million, with a length of 1000 nm -it can stretch to 3000 nm! Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham The Sequence of Amino Acids in a Protein • is a unique characteristic of every protein • is encoded by the nucleotide sequence of DNA • is thus a form of genetic information • is read from the amino terminus to the carboxyl terminus Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham The sequence of ribonuclease A Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham 5.2 Architecture of Proteins • Shape - globular or fibrous • The levels of protein structure - Primary - sequence - Secondary - local structures - H-bonds - Tertiary - overall 3-dimensional shape - Quaternary - subunit organization Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham What forces determine the structure? • Primary structure - determined by covalent bonds • Secondary, Tertiary, Quaternary structures all determined by weak forces • Weak forces - H-bonds, ionic interactions, van der Waals interactions, hydrophobic interactions Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham How to view a protein? • • • • backbone only backbone plus side chains ribbon structure space-filling structure Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Configuration and conformation are not the same Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham 5.3 Biological Functions of Proteins • • • • • • Proteins are the agents of biological function Enzymes - Ribonuclease Regulatory proteins - Insulin Transport proteins - Hemoglobin Structural proteins - Collagen Contractile proteins - Actin, Myosin Exotic proteins - Antifreeze proteins in fish Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham The tetrameric structure of hemoglobin Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham 5.4 Other Chemical Groups in Proteins Proteins may be "conjugated" with other chemical groups • If the non-amino acid part of the protein is important to its function, it is called a prosthetic group. • Be familiar with the terms: glycoprotein, lipoprotein, nucleoprotein, phosphoprotein, metalloprotein, hemoprotein, flavoprotein. Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham 5.7 Sequence Determination Frederick Sanger was the first - in 1953, he sequenced the two chains of insulin. • Sanger's results established that all of the molecules of a given protein have the same sequence. • Proteins can be sequenced in two ways: - real amino acid sequencing - sequencing the corresponding DNA in the gene Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Insulin consists of two polypeptide chains, A and B, held together by two disulfide bonds. The A chain has 21 residues and the B chain has 30 residues. The sequence shown is that of bovine insulin. Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Determining the Sequence An Eight Step Strategy • 1. If more than one polypeptide chain, separate. • 2. Cleave (reduce) disulfide bridges • 3. Determine composition of each chain • 4. Determine N- and C-terminal residues Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Determining the Sequence An Eight Step Strategy • 5. Cleave each chain into smaller fragments and determine the sequence of each chain • 6. Repeat step 5, using a different cleavage procedure to generate a different set of fragments. Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Determining the Sequence An Eight Step Strategy • 7. Reconstruct the sequence of the protein from the sequences of overlapping fragments • 8. Determine the positions of the disulfide crosslinks Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Step 1: Separation of chains • Subunit interactions depend on weak forces • Separation is achieved with: - extreme pH - 8M urea - 6M guanidine HCl - high salt concentration (usually ammonium sulfate) Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Step 2: Cleavage of Disulfide bridges • Performic acid oxidation • Sulfhydryl reducing agents - mercaptoethanol - dithiothreitol or dithioerythritol - to prevent recombination, follow with an alkylating agent like iodoacetate Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Step 3: Determine Amino Acid Composition • described on pages 112,113 of G&G • results often yield ideas for fragmentation of the polypeptide chains (Step 5, 6) Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Step 4: Identify N- and C-terminal residues • N-terminal analysis: – – – – Edman's reagent phenylisothiocyanate derivatives are phenylthiohydantions or PTH derivatives Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Step 4: Identify N- and C-terminal residues • C-terminal analysis – Enzymatic analysis (carboxypeptidase) – Carboxypeptidase A cleaves any residue except Pro, Arg, and Lys – Carboxypeptidase B (hog pancreas) only works on Arg and Lys Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Steps 5 and 6: Fragmentation of the chains • Enzymatic fragmentation – trypsin, chymotrypsin, clostripain, staphylococcal protease • Chemical fragmentation – cyanogen bromide Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Enzymatic Fragmentation • Trypsin - cleavage on the C-side of Lys, Arg • Chymotrypsin - C-side of Phe, Tyr, Trp • Clostripain - like trypsin, but attacks Arg more than Lys • Staphylococcal protease – C-side of Glu, Asp in phosphate buffer – specific for Glu in acetate or bicarbonate buffer Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Chemical Fragmentation • • • • Cyanogen bromide CNBr acts only on methionine residues CNBr is useful because proteins usually have only a few Met residues see Fig. 5.21 for mechanism be able to recognize the results! – a peptide with a C-terminal homoserine lactone Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Step 7: Reconstructing the Sequence • Use two or more fragmentation agents in separate fragmentation experiments • Sequence all the peptides produced (usually by Edman degradation) • Compare and align overlapping peptide sequences to learn the sequence of the original polypeptide chain Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Reconstructing the Sequence Compare cleavage by trypsin and staphylococcal protease on a typical peptide: • Trypsin cleavage: A-E-F-S-G-I-T-P-K L-V-G-K • Staphylococcal protease: F-S-G-I-T-P-K L-V-G-K-A-E Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Reconstructing the Sequence • The correct overlap of fragments: L-V-G-K A-E-F-S-G-I-T-P-K L-V-G-K-A-E F-S-G-I-T-P-K • Correct sequence: L-V-G-K-A-E-F-S-G-I-T-P-K Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Sequence analysis of catrocollastatin-C, a 23.6 kD protein from the venom of Crotalus atrox Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Nature of Protein Sequences • Sequences and composition reflect the function of the protein • Membrane proteins have more hydrophobic residues, whereas fibrous proteins may have atypical sequences • Homologous proteins from different organisms have homologous sequences • e.g., cytochrome c is highly conserved Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Phylogeny of Cytochrome c • The number of amino acid differences between two cytochrome c sequences is proportional to the phylogenetic difference between the species from which they are derived • This observation can be used to build phylogenetic trees of proteins • This is the basis for studies of molecular evolution Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Laboratory Synthesis of Peptides • Strategies are complex because of the need to control side chain reactions • Blocking groups must be added and later removed • du Vigneaud’s synthesis of oxytocin in 1953 was a milestone • Bruce Merrifield’s solid phase method was even more significant Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Solid Phase Synthesis • Carboxy terminus of a nascent peptide is covalently anchored to an insoluble resin • After each addition of a residue, the resin particles are collected by filtration • Automation and computer control now permit synthesis of peptides of 30 residues or more Copyright © 1999 by Harcourt Brace & Company Biochemistry 2/e - Garrett & Grisham Copyright © 1999 by Harcourt Brace & Company