Rapid Chemical Synthesis of Serine Protease Inhibitor Kazal-type 13 (SPINK13) Glycoform by a Combined Method with Glycan Insertion Strategy and Fast-Flow Fmoc SPPS.


Journal

Chemistry (Weinheim an der Bergstrasse, Germany)
ISSN: 1521-3765
Titre abrégé: Chemistry
Pays: Germany
ID NLM: 9513783

Informations de publication

Date de publication:
26 Jul 2023
Historique:
received: 28 02 2023
medline: 27 7 2023
pubmed: 9 6 2023
entrez: 9 6 2023
Statut: ppublish

Résumé

Serine protease inhibitor Kazal type 13 (SPINK13) is a secreted protein that has been recently studied as a therapeutic drug and an interesting biomarker for cancer cells. Although SPINK13 has a consensus sequence (Pro-Asn-Val-Thr) for N-glycosylation, the existence of N-glycosylation and its functions are still unclear. In addition to this, the preparation of glycosylated SPINK 13 has not been examined by both the cell expression method and chemical synthesis. Herein we report the chemical synthesis of the scarce N-glycosylated form of SPINK13 by a rapid synthetic method combined with the chemical glycan insertion strategy and a fast-flow SPPS method. Glycosylated asparagine thioacid was designed to chemoselectively be inserted between two peptide segments where is the sterically bulky Pro-Asn(N-glycan)-Val junction by two coupling reactions which consist of diacyl disulfide coupling (DDC) and thioacid capture ligation (TCL). This insertion strategy successfully afforded the full-length polypeptide of SPINK13 within two steps from glycosylated asparagine thioacid. Because the two peptides used for this synthesis were prepared by a fast-flow SPPS, the total synthetic time of glycoprotein was considerably shortened. This synthetic concept enables us to repetitively synthesize a target glycoprotein easily. Folding experiments afforded well-folded structure confirmed by CD and disulfide bond map. Invasion assays of glycosylated SPINK13 and non-glycosylated SPINK13 with pancreatic cancer cells showed that non-glycosylated SPINK-13 was more potent than that of glycosylated SPINK13.

Identifiants

pubmed: 37294165
doi: 10.1002/chem.202300646
doi:

Substances chimiques

Serine Proteinase Inhibitors 0
Asparagine 7006-34-0
stable plasma protein solution 0
Peptides 0
Glycoproteins 0
Polysaccharides 0
Disulfides 0

Types de publication

Journal Article

Langues

eng

Sous-ensembles de citation

IM

Pagination

e202300646

Subventions

Organisme : Japan Society for the Promotion of Science
ID : 17H01214, 21H05028, 21H04708
Organisme : Japan Society for the Promotion of Science
ID : 20J20649
Organisme : Mizutani Foundation for Glycoscience
ID : 210074

Informations de copyright

© 2023 Wiley-VCH GmbH.

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Auteurs

Kota Nomura (K)

Department of Chemistry, Graduate School of Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka, 560-0043, Japan.

Ryo Okamoto (R)

Department of Chemistry, Graduate School of Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka, 560-0043, Japan.
Forefront Research Center, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka, 560-0043, Japan.

Yuta Maki (Y)

Department of Chemistry, Graduate School of Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka, 560-0043, Japan.
Forefront Research Center, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka, 560-0043, Japan.

Ayumu Hayashibara (A)

Department of Molecular Biochemistry and Clinical Investigation, Graduate School of Medicine, Osaka University, 1-7 Yamadaoka, Suita, Osaka, 565-0871, Japan.

Toshifumi Takao (T)

Institute of Protein Research, Osaka University, 3-2, Yamadaoka, Suita, Osaka, 565-0871, Japan.

Tomoya Fukuoka (T)

Department of Molecular Biochemistry and Clinical Investigation, Graduate School of Medicine, Osaka University, 1-7 Yamadaoka, Suita, Osaka, 565-0871, Japan.

Eiji Miyoshi (E)

Department of Molecular Biochemistry and Clinical Investigation, Graduate School of Medicine, Osaka University, 1-7 Yamadaoka, Suita, Osaka, 565-0871, Japan.

Bradley L Pentelute (BL)

Department of Chemistry, Massachusetts Institute of Technology B18, R596, 77 Massachusetts Ave., Cambridge, MA 02139, USA.

Yasuhiro Kajihara (Y)

Department of Chemistry, Graduate School of Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka, 560-0043, Japan.
Forefront Research Center, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka, 560-0043, Japan.

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