Zhou Dongmei, Wang Xianxia, Zou Jun, Song Jiayi, Su Ping, Yang Yi, Wu Liqing
National Institute of Metrology, P.R. China, No. 18, North Third Ring East Road, Beijing, China.
China Quality Certification Centre, Building 3, Zone 9, No. 188, South Fourth Ring West Road, Fengtai District, Beijing, China.
Anal Methods. 2024 Mar 22;16(12):1741-1747. doi: 10.1039/d3ay02114a.
The present work assessed the purity of [Glu]-fibrinopeptide B (GFB) as a model peptide using gas chromatography - isotope dilution mass spectrometry. GFB and various isotope-labeled amino acids were hydrolyzed in HCl and then derivatized using optimized procedures. The primary impurity in GFB was also identified and used to correct the final result. A method repeatability of 0.5% was achieved and linear calibrations were obtained for five amino acids. The LOD and LOQ were 0.041 to 0.096 μg g, and 0.16 to 0.56 μg g, respectively. The purity of GFB was found to be (0.715 ± 0.012) g g. This technique exhibited comparable accuracy to that obtainable from liquid chromatography - isotope dilution mass spectrometry but at lower cost. This method could be employed as a reference technique or in fields such as clinical diagnostics or bio-pharmaceutical peptide purity analysis.
本研究采用气相色谱-同位素稀释质谱法评估了作为模型肽的[Glu]-纤维蛋白肽B（GFB）的纯度。GFB和各种同位素标记的氨基酸在盐酸中水解，然后采用优化程序进行衍生化。还鉴定了GFB中的主要杂质，并用于校正最终结果。方法重复性达到0.5%，获得了五种氨基酸的线性校准曲线。检测限和定量限分别为0.041至0.096μg/g和0.16至0.56μg/g。发现GFB的纯度为(0.715±0.012)g/g。该技术表现出与液相色谱-同位素稀释质谱法相当的准确度，但成本更低。该方法可作为参考技术，或用于临床诊断或生物制药肽纯度分析等领域。
