Haselberg Rob, de Jong Gerhardus J, Somsen Govert W
Department of Biomedical Analysis, Utrecht University, Utrecht, The Netherlands.
J Sep Sci. 2009 Jul;32(14):2408-15. doi: 10.1002/jssc.200900164.
The usefulness of a noncovalent, positively charged capillary coating for the efficient analysis of intact basic proteins with CE was studied. Capillaries were coated by subsequent flushing with solutions of 10% w/v Polybrene (PB), 3% w/v dextran sulfate (DS), and again 10% w/v PB. Coating characterization studies showed that stable coatings could be produced which exhibited a pH-independent and highly reproducible EOF. The PB-DS-PB coating was evaluated with Tris phosphate BGEs of various pH using the four basic model proteins: alpha-chymotrypsinogen A, ribonuclease A, cytochrome c, and lysozyme. Typical migration time RSDs for the proteins were less than 0.85%, and apparent plate numbers were above 125,000 using a capillary length of 40 cm. The high separation efficiency allowed detection of several minor impurities in the model proteins. Using a BGE of medium pH, the CE system with triple-layer coating appeared to be useful for the repeatable profiling of recombinant humanized mouse monoclonal immunoglobulin G(1) showing a characteristic pattern of glycoforms. The CE system was also applied to the characterization of two llama antibodies, which were produced in Saccharomyces cerevisiae, revealing the presence of a side product in one of the antibodies. The high migration time stability allowed the reliable determination of antibody-antigen binding by monitoring migration time shifts. Finally, the feasibility of using the PB-DS-PB coated capillaries for CE with mass spectrometric detection was shown by the characterization of the impure llama antibody sample.
研究了一种用于毛细管电泳(CE)高效分析完整碱性蛋白质的非共价带正电毛细管涂层的实用性。通过依次用10% (w/v)聚凝胺(PB)溶液、3% (w/v)硫酸葡聚糖(DS)溶液冲洗,然后再用10% (w/v)PB溶液冲洗来对毛细管进行涂层处理。涂层表征研究表明,可以制备出稳定的涂层,其表现出与pH无关且高度可重复的电渗流(EOF)。使用四种碱性模型蛋白:α-胰凝乳蛋白酶原A、核糖核酸酶A、细胞色素c和溶菌酶,对PB-DS-PB涂层在不同pH值的磷酸三乙胺背景电解质(BGE)中进行了评估。使用40 cm长的毛细管时,蛋白质的典型迁移时间相对标准偏差(RSD)小于0.85%,表观塔板数超过125,000。高分离效率使得能够检测模型蛋白中的几种次要杂质。使用中等pH值的BGE时,具有三层涂层的CE系统似乎可用于重组人源化小鼠单克隆免疫球蛋白G(1)的可重复分析,显示出糖型的特征模式。该CE系统还应用于两种在酿酒酵母中产生的骆驼抗体的表征,揭示了其中一种抗体中存在副产物。高迁移时间稳定性使得通过监测迁移时间变化能够可靠地测定抗体 - 抗原结合。最后,通过对不纯的骆驼抗体样品进行表征,证明了使用PB-DS-PB涂层毛细管进行CE与质谱检测联用的可行性。