Abstract
The total chemical synthesis of proteins has great potential for increasing our understanding of the molecular basis of protein function. The introduction of native chemical ligation techniques to join unprotected peptides next to a cysteine residue has greatly facilitated the synthesis of proteins of moderate size. Here, we describe a straightforward methodology that has enabled us to rapidly analyze the compatibility of the native chemical ligation strategy for X-Cys ligation sites, where X is any of the 20 naturally occurring amino acids. The simplified methodology avoids the necessity of specific amino acid thioester linkers or alkylation of C-terminal thioacid peptides. Experiments using matrix-assisted laser-desorption ionization MS analysis of combinatorial ligations of LYRAX-C-terminal thioester peptides to the peptide CRANK show that all 20 amino acids are suitable for ligation, with Val, Ile, and Pro representing less favorable choices because of slow ligation rates. To illustrate the method's utility, two 124-aa proteins were manually synthesized by using a three-step, four-piece ligation to yield a fully active human secretory phospholipase A(2) and a catalytically inactive analog. The combination of flexibility in design with general access because of simplified methodology broadens the applicability and versatility of chemical protein synthesis.
MeSH Terms
Amino Acid Sequence
Amino Acids, Sulfur
Chemistry, Organic/methods
Cysteine
Humans
Indicators and Reagents
Kinetics
Molecular Sequence Data
Peptide Fragments/chemistry
Peptides/chemical synthesis,chemistry
Phospholipases A/chemical synthesis,chemistry
Proteins/chemical synthesis,chemistry
Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization
Chemicals
Amino Acids, Sulfur
Indicators and Reagents
Peptide Fragments
Peptides
Proteins
Phospholipases A
Cysteine
Authors & Affiliations
3 authors, click to expand affiliations / ORCID
Hackeng T M
Department of Molecular and Experimental Medicine, The Scripps Research Institute, La Jolla, CA 92037, USA.
Griffin J H
Dawson P E
References (23)
23 references, click to expand
-
Peptide segment coupling in aqueous medium: silver ion activation of the thiolcarboxyl group.
Int J Pept Protein Res. 1981 Feb;17(2):273-4
PMID: 7228502
-
Semisynthesis of cytotoxic proteins using a modified protein splicing element.
Protein Sci. 1998 Nov;7(11):2256-64
PMID: 9827992
-
Chiral synthesis of a dithiolester analog of phosphatidylcholine as a substrate for the assay of phospholipase A2.
J Lipid Res. 1983 Nov;24(11):1532-7
PMID: 6655369
-
Structure-function relationships of phospholipases. The anticoagulant region of phospholipases A2.
J Biol Chem. 1987 Oct 25;262(30):14402-7
PMID: 3117784
-
Chemical synthesis of peptides and proteins.
Annu Rev Biochem. 1988;57:957-89
PMID: 3052294
-
A general method for site-specific incorporation of unnatural amino acids into proteins.
Science. 1989 Apr 14;244(4901):182-8
PMID: 2649980
-
Effect of reducing disulfide-containing proteins on electrospray ionization mass spectra.
Anal Chem. 1990 Apr 1;62(7):693-8
PMID: 2327585
-
Purification and characterization of a mutant human platelet phospholipase A2 expressed in Escherichia coli. Cleavage of a fusion protein with cyanogen bromide.
Eur J Biochem. 1992 Jan 15;203(1-2):89-98
PMID: 1730245
-
Analysis of human synovial fluid phospholipase A2 on short chain phosphatidylcholine-mixed micelles: development of a spectrophotometric assay suitable for a microtiterplate reader.
Anal Biochem. 1992 Jul;204(1):190-7
PMID: 1514686
-
In situ neutralization in Boc-chemistry solid phase peptide synthesis. Rapid, high yield assembly of difficult sequences.
Int J Pept Protein Res. 1992 Sep-Oct;40(3-4):180-93
PMID: 1478777
-
Diversity of group types, regulation, and function of phospholipase A2.
J Biol Chem. 1994 May 6;269(18):13057-60
PMID: 8175726
-
Determinants of the inhibitory action of purified 14-kDa phospholipases A2 on cell-free prothrombinase complex.
J Biol Chem. 1994 Oct 21;269(42):26338-43
PMID: 7929351
-
Synthesis of proteins by native chemical ligation.
Science. 1994 Nov 4;266(5186):776-9
PMID: 7973629
-
Peptide synthesis using unprotected peptides through orthogonal coupling methods.
Proc Natl Acad Sci U S A. 1995 Dec 19;92(26):12485-9
PMID: 8618926
-
The anticoagulant effect of the human secretory phospholipase A2 on blood plasma and on a cell-free system is due to a phospholipid-independent mechanism of action involving the inhibition of factor Va.
Eur J Biochem. 1996 May 1;237(3):778-85
PMID: 8647125
-
Life with 6000 genes.
Science. 1996 Oct 25;274(5287):546, 563-7
PMID: 8849441
-
The mechanism of protein splicing and its modulation by mutation.
EMBO J. 1996 Oct 1;15(19):5146-53
PMID: 8895558
-
The leucine zipper domain controls the orientation of AP-1 in the NFAT.AP-1.DNA complex.
Chem Biol. 1996 Dec;3(12):981-91
PMID: 9000009
-
Total chemical synthesis of enzymatically active human type II secretory phospholipase A2.
Proc Natl Acad Sci U S A. 1997 Jul 22;94(15):7845-50
PMID: 9223275
-
Protein synthesis by chemical ligation of unprotected peptides in aqueous solution.
Methods Enzymol. 1997;289:266-98
PMID: 9353726
-
Chemical ligation of unprotected peptides directly from a solid support.
J Pept Res. 1998 Apr;51(4):303-16
PMID: 9560006
-
Expressed protein ligation: a general method for protein engineering.
Proc Natl Acad Sci U S A. 1998 Jun 9;95(12):6705-10
PMID: 9618476
-
Quantitative monitoring of solid-phase peptide synthesis by the ninhydrin reaction.
Anal Biochem. 1981 Oct;117(1):147-57
PMID: 7316187