Bio Therapeutics Development, Janssen Research & Development, LLC , Malvern , PA , USA.
MAbs. 2019 Oct;11(7):1233-1244. doi: 10.1080/19420862.2019.1646554. Epub 2019 Sep 2.
In recent years, capillary electrophoresis-sodium dodecyl sulfate (cSDS) has been widely used for high resolution separation and quantification of the fragments and aggregates of monoclonal antibodies (mAbs) to ensure the quality of mAb therapeutics. However, identification of the low-molecular-weight (LMW) and high-molecular-weight (HMW) species detected in cSDS electropherograms has been based primarily on the approximate MWs calculated from standard curves using known MW standards and correlations with fragments and aggregates identified by other methods. It is not easy to collect sufficient amounts of H/LMW species from cSDS for analysis by orthogonal methods and the direct coupling of cSDS with mass spectrometry (MS) is very difficult due to interference from SDS. In this study, we describe the precise identification of H/LMW species detected by cSDS using reversed-phase high performance liquid chromatography (RP-HPLC) coupled with top-down tandem MS analysis. The H/LMW species were first identified by on-line RP-HPLC MS analysis and the RP-HPLC fractions were then analyzed by cSDS to connect the identified H/LMW species with the peaks in the cSDS electropherogram. With this method, 58 unique H/LMW species were identified from an immunoglobulin G1 (IgG1) mAb. The identified fragments ranged from 10 kDa single chain fragments to 130 kDa triple chain fragments, including some with post-translational modifications. This is the first study to clearly identify the antibody fragments, including the exact clipping sites, observed in cSDS electropherograms. The methodology and results presented here should be applicable to most other IgG1 mAbs.
近年来,毛细管电泳-十二烷基硫酸钠(cSDS)已广泛用于单克隆抗体(mAb)片段和聚集体的高分辨率分离和定量,以确保 mAb 治疗药物的质量。然而,cSDS 电泳图谱中检测到的低分子量(LMW)和高分子量(HMW)物质的鉴定主要基于从标准曲线计算的近似分子量,这些标准曲线使用已知分子量标准品和与其他方法鉴定的片段和聚集体的相关性。从 cSDS 中收集足够量的 H/LMW 物质用于正交方法分析并不容易,并且由于 SDS 的干扰,cSDS 与质谱(MS)的直接耦合非常困难。在这项研究中,我们描述了使用反相高效液相色谱(RP-HPLC)与自上而下串联 MS 分析相结合,对 cSDS 检测到的 H/LMW 物质进行精确鉴定。首先通过在线 RP-HPLC-MS 分析鉴定 H/LMW 物质,然后用 cSDS 分析 RP-HPLC 馏分,将鉴定的 H/LMW 物质与 cSDS 电泳图谱中的峰连接起来。使用这种方法,从免疫球蛋白 G1(IgG1)mAb 中鉴定出 58 种独特的 H/LMW 物质。鉴定出的片段范围从 10 kDa 单链片段到 130 kDa 三链片段,包括一些具有翻译后修饰的片段。这是首次明确鉴定 cSDS 电泳图谱中观察到的抗体片段,包括确切的剪接位点。这里提出的方法和结果应该适用于大多数其他 IgG1 mAb。