Natarajan Arutselvan, Xiong Cheng-Yi, Albrecht Huguette, DeNardo Gerald L, DeNardo Sally J
University of California Davis Medical Center, Sacramento, California 95816, USA.
Bioconjug Chem. 2005 Jan-Feb;16(1):113-21. doi: 10.1021/bc0498121.
New radiopharmaceuticals are possible using site-specific conjugation of small tumor binding proteins and poly(ethylene glycol) (PEG) scaffolds to provide modular multivalent, homo- or heterofunctional cancer-targeting molecules having preferred molecular size, valence, and functionality. Residence time in plasma can be optimized by modification of the size, number, and charge of the protein units. However, random PEG conjugation (PEGylation) of these small molecules via amine groups has led to variations of structural conformation and binding affinity. To optimize PEGylation, scFvs have been recombinantly produced in a vector that adds an unpaired cysteine (c) near the scFv carboxy terminus (scFv-c), thus providing a specific site for thiol conjugation. To evaluate the general applicability of this unpaired cysteine for PEGylation of scFv-c, conjugation efficiency was determined for four different scFvs and several PEG molecules having thiol reactive groups. The effect of the PEG molecular format on scFv-c PEG malignant cell binding was also addressed. ScFvs produced as scFv-c and purified by anti E-TAG affinity chromatography were conjugated using PEG molecules with maleimide (Mal) or o-pyridyl disulfide (OPSS). Conjugations were performed at pH 7.0, with 2 molar excess TCEP/scFv and PEG-(Mal) or PEG-OPSS, using 5:1 (PEG/scFv). PEG-Mal conjugation efficiency was also evaluated with 1:5 (PEG/scFv). PEGylation efficiency was determined for each reaction by quantitation of the products on SDS-PAGE. ScFv-c conjugation with unifunctional maleimide PEGs resulted in PEG conjugates incorporating 30-80% of the scFv-c, but usually above 50%. Efficiency of scFv-c conjugation to both functional groups of the bifunctional PEG-(Mal)2 varied between the PEG and scFv-c molecules studied. A maximum of 45% of scFv-c protein was conjugated as PEG- (scFv-c)2 using the smallest PEG-(Mal)2 (2 kDa). No significant increase in scFv-c conjugation was observed by the use of greater than a 5 molar excess of PEG/scFv-c. Under the same conjugation conditions, PEG as OPSS yielded less than 10% PEG-scFv-c. PEG-(scFv)2 conjugates had increased binding in ELISA using malignant cell membranes, when compared with unmodified scFv-c. PEGylated-scFv binding was comparable with unmodified scFv-c. In summary, scFv-c can be PEGylated in a site-specific manner using uni- or bivalent PEG-Mal, either linear or branched. ScFv-c was most efficiently conjugated to smaller PEG-Mal molecules, with the smallest, 2 kDa PEG-Mal, usually PEGylating 60-90% of the scFv-c. ScFv-c conjugation to form PEG-(scFv-c)2 reached greatest efficiency at 45%, and its purified form demonstrated greater binding than the corresponding scFv-c.
利用小肿瘤结合蛋白与聚乙二醇(PEG)支架进行位点特异性缀合,从而提供具有优选分子大小、价态和功能的模块化多价、同功能或异功能癌症靶向分子,新型放射性药物成为可能。通过修饰蛋白质单元的大小、数量和电荷,可以优化其在血浆中的停留时间。然而,这些小分子通过胺基进行的随机PEG缀合(PEG化)导致了结构构象和结合亲和力的变化。为了优化PEG化,单链抗体片段(scFv)已在载体中重组产生,该载体在scFv羧基末端附近添加了一个未配对的半胱氨酸(c)(scFv-c),从而为硫醇缀合提供了一个特定位点。为了评估这种未配对半胱氨酸对scFv-c进行PEG化的普遍适用性,测定了四种不同scFv与几种具有硫醇反应性基团的PEG分子的缀合效率。还研究了PEG分子形式对scFv-c与恶性细胞结合的影响。以scFv-c形式产生并通过抗E-TAG亲和色谱法纯化的scFv,使用带有马来酰亚胺(Mal)或邻吡啶二硫(OPSS)的PEG分子进行缀合。缀合在pH 7.0条件下进行,TCEP/scFv和PEG-(Mal)或PEG-OPSS的摩尔过量为2,PEG与scFv的比例为5:1。也用1:5(PEG/scFv)评估了PEG-Mal缀合效率。通过SDS-PAGE对产物进行定量,确定每个反应的PEG化效率。单功能马来酰亚胺PEG与scFv-c的缀合产生了包含30-80% scFv-c的PEG缀合物,但通常高于50%。在研究的PEG和scFv-c分子中,双功能PEG-(Mal)2的两个功能基团与scFv-c的缀合效率各不相同。使用最小的PEG-(Mal)2(2 kDa)时,最多45%的scFv-c蛋白被缀合为PEG-(scFv-c)2。使用大于5摩尔过量PEG/scFv-c未观察到scFv-c缀合的显著增加。在相同的缀合条件下,以OPSS形式存在的PEG产生的PEG-scFv-c少于10%。与未修饰的scFv-c相比,PEG-(scFv)2缀合物在使用恶性细胞膜的ELISA中结合增加。PEG化-scFv的结合与未修饰的scFv-c相当。总之,scFv-c可以使用单价或二价的线性或分支PEG-Mal以位点特异性方式进行PEG化。scFv-c与最小的2 kDa PEG-Mal这种较小的PEG-Mal分子缀合效率最高,通常60-90%的scFv-c被PEG化。形成PEG-(scFv-c)2的scFv-c缀合效率最高可达45%,其纯化形式显示出比相应scFv-c更强的结合能力。