Vaidyanathan G, Zalutsky M R
Department of Radiology, Duke University Medical Center, Durham, North Carolina 27710.
Bioconjug Chem. 1994 Jul-Aug;5(4):352-6. doi: 10.1021/bc00028a012.
Our previously reported method for the 18F labeling of antibodies using N-succinimidyl 4-[18F]fluorobenzoate (SFB) involved a rather long synthesis time. Here we present an improved method for the synthesis of SFB which reduces the synthesis time by about 45 min. A reaction time of 5-8 min (versus 25 min for the original procedure) was sufficient in the fluorination step to form 4-[18F]fluorobenzaldehyde in high yield. In the original method, 30-35 min was necessary to convert 4-[18F]fluorobenzoic acid to SFB using dicyclohexylcarbodiimide and N-hydroxysuccinimide. When N,N'-disuccinimidyl carbonate was used, facile conversion of 4-fluorobenzoic acid to SFB was seen at a micromolar level. At a tracer level, no product was formed at room temperature; however, complete consumption of starting material was observed. Heating at 150 degrees C resulted in the formation of SFB in more than 80% yield in 1-3 min. HPLC purification of SFB was necessary since use of crude SFB, or SFB purified using a silica solid-phase cartridge column, resulted in lower protein coupling yields. Furthermore, use of crude SFB resulted in cross-linking and lower immunoreactivity of antibody. Largely as a result of the considerable reduction in total labeling time, these modifications have increased the amount of 18F-labeled antibody available per 100 mCi of [18F]fluoride by 30-35%.
我们之前报道的使用N-琥珀酰亚胺基4-[¹⁸F]氟苯甲酸酯(SFB)对抗体进行¹⁸F标记的方法合成时间相当长。在此,我们提出一种改进的SFB合成方法,该方法将合成时间缩短了约45分钟。氟化步骤中5 - 8分钟的反应时间(原方法为25分钟)足以高产率地生成4-[¹⁸F]氟苯甲醛。在原方法中,使用二环己基碳二亚胺和N-羟基琥珀酰亚胺将4-[¹⁸F]氟苯甲酸转化为SFB需要30 - 35分钟。当使用N,N'-二琥珀酰亚胺基碳酸酯时,在微摩尔水平上可轻松将4-氟苯甲酸转化为SFB。在示踪剂水平下,室温下不形成产物;然而,观察到起始原料完全消耗。在150℃加热1 - 3分钟可使SFB的产率超过80%。由于需要对SFB进行HPLC纯化,因为使用粗制SFB或使用硅胶固相柱纯化的SFB会导致较低的蛋白质偶联产率。此外,使用粗制SFB会导致抗体交联并降低免疫反应性。总体而言,由于总标记时间大幅减少,这些改进使每100毫居里[¹⁸F]氟化物可得的¹⁸F标记抗体量增加了30 - 35%。