Radiolabeled peptide synthesis and characterization

All chemicals and solvents were obtained from commercial suppliers and were used without further purification, unless specified. Lutetium-177 (LuMark Lutetium-177 chloride) was purchased from IDB Holland (Baarle-Nassau, The Netherlands) and indium-111 (Indium (In-111) chloride) was purchased from Curium Netherlands BV (Petten, The Netherlands). HTK01169 and its derivatives were synthesized by solid-phase peptide synthesis (SPPS), with the exception of certain steps performed in liquid phase, as specified below. Reactions were monitored by thin-layer chromatography (TLC) using silica gel 60 F254 plates (Merck; Darmstadt, Germany) and visualized under ultraviolet light or by staining with 10% phosphomolybdic acid in ethanol. Solid-phase reactions were monitored by Kaiser test. Liquid chromatography–mass spectrometry (LC-MS) analyses were performed on an Agilent 1260 Infinity II LC/MSD XT system (Amstelveen, The Netherlands) controlled by ChemStation software. Nuclear magnetic resonance (NMR) spectra were recorded in CDCl₃ and CD₃OD on a Bruker Ascend 600 MHz system (Leiderdorp, The Netherlands) at ambient temperature. Chemical shifts are given as δ values in ppm and coupling constants J are given in Hz. The splitting patterns are reported as s (singlet), d (doublet), t (triplet), m (multiplet), dd (doublet of doublets) and br (broad signal). Reverse-phase high-performance liquid chromatography (RP-HPLC) was performed with a Waters Alliance e2695 system (Etten-Leur, The Netherlands) equipped with a 2998 diode array (PDA) detector, a NaI(Tl) Scionix crystal (Bunnik, The Netherlands) connected to a Canberra Osprey multichannel analyzer and signal amplifier (Zellik, Belgium), and Empower 3 software. Radioactivity was measured using a PerkinElmer Wizard 2 γ-counter (Groningen, The Netherlands). Instant thin-layer iTLC-SG chromatography plates (Agilent; Folsom, CA, USA) were analysed by radio-chromatography with a bSCAN scanner (Brightspec; Antwerp, Belgium). Radiochemical yield (RCY), expressed as a percentage (%), is determined by iTLC and corresponds to the ratio of the peak area of the radiolabelled product and the peak area of all radiochemical species. Radiochemical purity (RCP), expressed as a percentage (%), corresponds to the ratio between the peak area of the radiolabelled product and the peak area of all radiochemical species integrated via radio-HPLC.

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Murce E., de Blois E., van den Berg S., de Jong M, & Seimbille Y. (2023). Synthesis and radiolabelling of PSMA-targeted derivatives containing GYK/MVK cleavable linkers. Royal Society Open Science, 10(3), 220950.

Publication 2023

Chloride Chromatography Curium Derivatives Ethanol Hplc In 111 Indium Liquid chromatography Lutetium 177 Mass spectrometry Nuclear magnetic resonance Phosphomolybdic acid Radioactivity Radiochemical Reverse phase liquid chromatography Silica gel Solvents Spps Thin layer chromatography Triplet Ultraviolet light

Corresponding Organization : TRIUMF

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Variable analysis

independent variables

Lutetium-177 (LuMark Lutetium-177 chloride)
Indium-111 (Indium (In-111) chloride)
HTK01169 and its derivatives

dependent variables

Radiochemical yield (RCY)
Radiochemical purity (RCP)

control variables

All chemicals and solvents were obtained from commercial suppliers and were used without further purification, unless specified.

positive controls

Not explicitly mentioned

negative controls

Not explicitly mentioned

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