Gupte Anshul, Wadhwa Saurabh, Mumper Russell J
Department of Pharmaceutical Sciences, College of Pharmacy, University of Kentucky, Lexington, Kentucky 40536-0082, USA.
Bioconjug Chem. 2008 Jul;19(7):1382-8. doi: 10.1021/bc800042s. Epub 2008 Jun 21.
D-Penicillamine (D-pen) is an established copper chelator. We have recently shown that the copper-catalyzed D-pen oxidation generates concentration-dependent hydrogen peroxide (H 2O 2). Additionally, D-pen coincubated with cupric sulfate resulted in cytotoxicity in human leukemia and breast cancer cells due to the extracellular generation of reactive oxygen species (ROS). The inherent physicochemical properties of D-pen such as its short in vivo half-life, low partition coefficient, and rapid metal catalyzed oxidation limit its intracellular uptake and the potential utility as an anticancer agent in vivo. Therefore, to enhance the intracellular delivery and to protect the thiol moiety of D-pen, we designed, synthesized, and evaluated a novel gelatin-D-pen conjugate. D-pen was covalently coupled to gelatin with a biologically reversible disulfide bond with the aid of a heterobifunctional cross-linker ( N-succinimidyl-3-(2-pyridyldithio)-propionate) (SPDP). Additionally, fluorescein-labeled gelatin-D-pen conjugate was synthesized for cell uptake studies. D-pen alone was shown not to enter leukemia cells. In contrast, the qualitative intracellular uptake of the conjugate in human leukemia cells (HL-60) was shown with confocal microscopy. The conjugate exhibited slow cell uptake (over the period of 48 to 72 h). A novel HPLC assay was developed to simultaneously quantify both D-pen and glutathione in a single run. The conjugate was shown to completely release D-pen in the presence of glutathione (1 mM) in approximately 3 h in PBS buffer, pH 7.4. The gelatin-D-pen conjugate resulted in significantly greater cytotoxicity compared to free D-pen, gelatin alone, and a physical mixture of gelatin and D-pen in human leukemia cells. Further studies are warranted to assess the potential of D-pen conjugate in the delivery of D-pen as a ROS generating anticancer agent.
D-青霉胺(D-pen)是一种公认的铜螯合剂。我们最近发现,铜催化的D-青霉胺氧化会产生浓度依赖性的过氧化氢(H₂O₂)。此外,D-青霉胺与硫酸铜共同孵育会导致人白血病和乳腺癌细胞产生细胞毒性,这是由于细胞外活性氧(ROS)的产生。D-青霉胺固有的物理化学性质,如体内半衰期短、分配系数低以及快速的金属催化氧化,限制了其细胞内摄取以及作为体内抗癌剂的潜在效用。因此,为了增强细胞内递送并保护D-青霉胺的硫醇部分,我们设计、合成并评估了一种新型的明胶-D-青霉胺共轭物。借助异双功能交联剂(N-琥珀酰亚胺基-3-(2-吡啶二硫基)-丙酸酯)(SPDP),D-青霉胺通过生物可逆的二硫键与明胶共价偶联。此外,还合成了荧光素标记的明胶-D-青霉胺共轭物用于细胞摄取研究。结果表明,单独的D-青霉胺不会进入白血病细胞。相比之下,通过共聚焦显微镜观察到共轭物在人白血病细胞(HL-60)中有定性的细胞内摄取。共轭物表现出缓慢的细胞摄取(在48至72小时内)。开发了一种新型的高效液相色谱法(HPLC),可在一次运行中同时定量D-青霉胺和谷胱甘肽。结果表明,在pH 7.4的PBS缓冲液中,共轭物在1 mM谷胱甘肽存在下约3小时内可完全释放D-青霉胺。与游离D-青霉胺、单独的明胶以及明胶和D-青霉胺的物理混合物相比,明胶-D-青霉胺共轭物在人白血病细胞中产生了显著更大的细胞毒性。有必要进行进一步的研究,以评估D-青霉胺共轭物作为产生ROS的抗癌剂递送D-青霉胺的潜力。