Goodin Jeremy L, Nellis David F, Powell Bradford S, Vyas Vinay V, Enama Jeffrey T, Wang Lena C, Clark Patrick K, Giardina Steven L, Adamovicz Jeffery J, Michiel Dennis F
Bacteriology Division, U.S. Army Medical Research Institute of Infectious Diseases, Fort Detrick, Frederick, MD 21702, USA.
Protein Expr Purif. 2007 May;53(1):63-79. doi: 10.1016/j.pep.2006.12.018. Epub 2006 Dec 31.
The F1-V vaccine antigen, protective against Yersinia pestis, exhibits a strong tendency to multimerize that affects larger-scale manufacture and characterization. In this work, the sole F1-V cysteine was replaced with serine by site-directed mutagenesis for characterization of F1-V non-covalent multimer interactions and protective potency without participation by disulfide-linkages. F1-V and F1-V(C424S) proteins were overexpressed in Escherichia coli, recovered using mechanical lysis/pH-modulation and purified from urea-solubilized soft inclusion bodies, using successive ion-exchange, ceramic hydroxyapatite, and size-exclusion chromatography. This purification method resulted in up to 2mg/g of cell paste of 95% pure, mono-disperse protein having < or =0.5 endotoxin units per mg by a kinetic chromogenic limulus amoebocyte lysate reactivity assay. Both F1-V and F1-V(C424S) were monomeric at pH 10.0 and progressively self-associated as pH conditions decreased to pH 6.0. Solution additives were screened for their ability to inhibit F1-V self-association at pH 6.5. An L-arginine buffer provided the greatest stabilizing effect. Conversion to >500-kDa multimers occurred between pH 6.0 and 5.0. Conditions for efficient F1-V adsorption to the cGMP-compatible alhydrogel adjuvant were optimized. Side-by-side evaluation for protective potency against subcutaneous plague infection in mice was conducted for F1-V(C424S) monomer; cysteine-capped F1-V monomer; cysteine-capped F1-V multimer; and a F1-V standard reported previously. After a two-dose vaccination with 2 x 20 microg of F1-V, respectively, 100%, 80%, 80%, and 70% of injected mice survived a subcutaneous lethal plague challenge with 10(8) LD(50)Y. pestis CO92. Thus, vaccination with F1-V monomer and multimeric forms resulted in significant, and essentially equivalent, protection.
对鼠疫耶尔森菌具有保护作用的F1-V疫苗抗原呈现出强烈的多聚化倾向,这影响了大规模生产和特性分析。在本研究中,通过定点诱变将F1-V唯一的半胱氨酸替换为丝氨酸,以表征F1-V的非共价多聚体相互作用和不涉及二硫键连接的保护效力。F1-V和F1-V(C424S)蛋白在大肠杆菌中过表达,采用机械裂解/pH调节法回收,并从尿素溶解的软包涵体中通过连续离子交换、陶瓷羟基磷灰石和尺寸排阻色谱法进行纯化。这种纯化方法每克细胞糊可得到高达2mg的95%纯的单分散蛋白,通过动力学显色鲎试剂反应性测定,每毫克蛋白的内毒素单位≤0.5。F1-V和F1-V(C424S)在pH 10.0时均为单体,随着pH条件降至pH 6.0,它们逐渐自我缔合。筛选了溶液添加剂在pH 6.5时抑制F1-V自我缔合的能力。L-精氨酸缓冲液提供了最大的稳定效果。在pH 6.0和5.0之间发生了向>500-kDa多聚体的转变。优化了F1-V与符合cGMP标准的氢氧化铝佐剂有效吸附的条件。对F1-V(C424S)单体、半胱氨酸封端的F1-V单体、半胱氨酸封端的F1-V多聚体以及先前报道的F1-V标准品进行了针对小鼠皮下鼠疫感染保护效力的平行评估。分别用2×20μg的F1-V进行两剂疫苗接种后,100%、80%、80%和70%的注射小鼠在接受10(8) LD(50)鼠疫耶尔森菌CO92的皮下致死性鼠疫攻击后存活。因此,用F1-V单体和多聚体形式进行疫苗接种产生了显著且基本等效的保护作用。