Oxford Antiviral Drug Discovery Unit, Oxford Glycobiology Institute, Department of Biochemistry, University of Oxford, South Parks Road, Oxford, OX1 3QU, United Kingdom.
Oxford University Hospitals NHS Foundation Trust, John Radcliffe Hospital, Headley Way, Headington, Oxford, OX3 9DU, United Kingdom.
Sci Rep. 2017 Sep 21;7(1):12072. doi: 10.1038/s41598-017-12229-2.
LC-MS and immunoassay can detect protein biomarkers. Immunoassays are more commonly used but can potentially be outperformed by LC-MS. These techniques have limitations including the necessity to generate separate calibration curves for each biomarker. We present a rapid mass spectrometry-based assay utilising a universal calibration curve. For the first time we analyse clinical samples using the HeavyPeptide IGNIS kit which establishes a 6-point calibration curve and determines the biomarker concentration in a single LC-MS acquisition. IGNIS was tested using apolipoprotein F (APO-F), a potential biomarker for non-alcoholic fatty liver disease (NAFLD). Human serum and IGNIS prime peptides were digested and the IGNIS assay was used to quantify APO-F in clinical samples. Digestion of IGNIS prime peptides was optimised using trypsin and SMART Digest™. IGNIS was 9 times faster than the conventional LC-MS method for determining the concentration of APO-F in serum. APO-F decreased across NAFLD stages. Inter/intra-day variation and stability post sample preparation for one of the peptides was ≤13% coefficient of variation (CV). SMART Digest™ enabled complete digestion in 30 minutes compared to 24 hours using in-solution trypsin digestion. We have optimised the IGNIS kit to quantify APO-F as a NAFLD biomarker in serum using a single LC-MS acquisition.
LC-MS 和免疫测定均可检测蛋白质生物标志物。免疫测定更为常用,但在性能上可能不如 LC-MS。这些技术存在局限性,包括需要为每个生物标志物生成单独的校准曲线。我们提出了一种基于快速质谱的检测方法,该方法利用通用校准曲线。我们首次使用 HeavyPeptide IGNIS 试剂盒分析临床样本,该试剂盒建立了 6 点校准曲线,并在单次 LC-MS 采集时确定生物标志物浓度。我们使用载脂蛋白 F (APO-F) 对 IGNIS 进行了测试,APO-F 是一种非酒精性脂肪性肝病 (NAFLD) 的潜在生物标志物。人血清和 IGNIS 起始肽被消化,然后使用 IGNIS 测定法在临床样本中定量 APO-F。使用胰蛋白酶和 SMART Digest™对 IGNIS 起始肽的消化进行了优化。与传统的 LC-MS 方法相比,IGNIS 测定法测定血清中 APO-F 浓度的速度快 9 倍。APO-F 在 NAFLD 各阶段均降低。其中一种肽的日内/日间变异和样品制备后稳定性的变异系数(CV)≤13%。与使用溶液中的胰蛋白酶消化相比,SMART Digest™ 可在 30 分钟内完成完全消化。我们已经优化了 IGNIS 试剂盒,以使用单次 LC-MS 采集来定量血清中的 APO-F 作为 NAFLD 生物标志物。