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@INPROCEEDINGS{Humpert:1027701,
author = {Humpert, Swen and Neumaier, Bernd and Zlatopolskiy, Boris},
title = {{C}onvenient preparation of 18{F}-labeled human insulin by
{P}d-catalyzed {S}-arylation},
issn = {0969-8051},
reportid = {FZJ-2024-04011},
year = {2022},
note = {This work was supported by the DFG grant ZL 65/4-1.},
abstract = {Objective: Insulin is a peptide hormone that is produced
andsecreted by pancreatic ß-cells. Apart from its
well-known role forthe regulation of blood glucose
homeostasis, insulin is consideredto be an important
modulator of certain brain functions, includingfeeding
behavior and cognition, although the mechanisms of insulin
transfer into the central nervous system (CNS) remain
unclear. Whilethe preparation of several radiolabeled
insulin derivatives has beenreported, their application as
probes for in vivo PET studies is hamperedby low yields and
low molar activities due to inefficient andlengthy
production routes. Herein we report a rapid and
efficientprocedure for the preparation of high molar
activity insulin selectivelylabeled at the Lys29 residue in
the B-chain.Methods: Radiolabeling of thiol-modified insulin
was performedby S-arylation with
2-[18F]Fluoro-5-iodopyridine ([18F]FIPy) in MeCN/phosphate
buffer at 37°C for 3 minutes in the presence of XantphosPd
G3 catalyst as recently reported [1]. The product was
isolated byRP HPLC with a conventional C18 column. The
appropriate substratefor S-conjugation was prepared as
follows. Treatment of humaninsulin with N-hydroxysuccimidyl
ester of S-Trt protected 4-mercaptobutyricacid in DMF/TRIS
buffer (pH = 10.5) afforded Lysb29acylated insulin, which
was deprotected with TFA/TIS/H2O (75:20:5).[18F]FIPy was
prepared from the corresponding DABCO precursorusing the
“minimalist” radiofluorination protocol and isolated by
SPEor fast HPLC (7 min).Results: Insulin containing an
SH-tag at the Lysb29 residue wasprepared in $14\%$ yield
over two steps. Subsequent conjugation withSPE-isolated
[18F]FIPy afforded the radiolabeled insulin derivative ina
RCY of $11\%$ over two steps. In contrast, conjugation of
HPLC-isolated[18F]FIPy with only 100–200 nmol
thiol-modified insulin yielded thedesired 18F-fluorinated
product in RCYs of 35 ± $4\%$ (n=4) with highradiochemical
and chemical purity within 60 min. The suitability forin
vivo PET studies was exemplified by preparation of 1.2 GBq
radiolabeledinsulin with a molar activity of 100 GBq/µmol
starting from6 GBq [18F]F−. Conclusion: Highly efficient
production of 18F-labeled insulin fromtiny precursor amounts
underlines the high potential of Pd-catalyzedS-arylation
with [18F]FIPy for radiolabeling of sensitive biomolecules.},
month = {May},
date = {2022-05-29},
organization = {24th International Symposium on
Radiopharmaceutical Sciences, Nantes
(France), 29 May 2022 - 3 Jun 2022},
subtyp = {After Call},
cin = {INM-5},
ddc = {570},
cid = {I:(DE-Juel1)INM-5-20090406},
pnm = {5253 - Neuroimaging (POF4-525)},
pid = {G:(DE-HGF)POF4-5253},
typ = {PUB:(DE-HGF)6},
doi = {10.1016/S0969-8051(22)00259-1},
url = {https://juser.fz-juelich.de/record/1027701},
}