Ye Cong, Xie Fei-Fei, Li Guo-Wei, Hu Qi-Ping, Tong Pei-Zhen, Wu Run-Song, Luo Wen-Hui, Sun Dong-Mei
Guangzhou University of Chinese Medicine Guangzhou 510006, China Guangdong Key Laboratory of Traditional Chinese Medicine Formula Granules, Guangdong Yifang Pharmaceutical Co., Ltd. Foshan 528244, China.
Guangdong Key Laboratory of Traditional Chinese Medicine Formula Granules, Guangdong Yifang Pharmaceutical Co., Ltd. Foshan 528244, China.
Zhongguo Zhong Yao Za Zhi. 2024 Jun;49(12):3185-3193. doi: 10.19540/j.cnki.cjcmm.20240216.102.
Peptidomics was employed to systematically analyze the characteristic peptides in Galli Gigerii Endothelium Corneum and its adulterants and establish a method for distinguishing Galli Gigerii Endothelium Corneum from its adulterants, including the gizzard membranes from ducks, geese, and pigeons. UPLC-Q-Exactive Orbitrap-MS was combined with multivariate statistical analysis to analyze the peptides in Galli Gigerii Endothelium Corneum and its adulterants. The structures of peptides were identified by pNovo combined with manual recognition of spectra, and synthetic peptide standards were used for validation. LC-MS/MS was used to optimize the sample pre-processing conditions, including the extraction procedure, extraction time, extraction solvents, and solvent volumes, for the characteristic peptide LESY in Galli Gigerii Endothelium Corneum. Multiple reaction monitoring(MRM) in the ESI+ mode with m/z 511.24→269.11 and 511.24→243.13 as detection ions was employed for qualitative and quantitative analyses. The established UPLC-MS/MS method demonstrated good specificity, stability, and durability. The content of LESY in 16 batches of Galli Gigerii Endothelium Corneum samples ranged from 55.03 to 113.36 μg·g(-1). Additionally, a qualitative detection method for the common peptide RDPVLVSR in adulterants was established with m/z 471.28→785.45 and 471.28→670.41 as the detection ions. This study established a convenient, rapid, and accurate detection method for the characteristic peptides in Galli Gigerii Endothelium Corneum and its adulterants. The method possesses good specificity, stability, and durability, providing a valuable reference for the identification and quality control of Galli Gigerii Endothelium Corneum and other traditional Chinese medicines derived from animal sources.
采用肽组学方法系统分析鸡内金及其掺伪品中的特征肽，并建立一种区分鸡内金与其掺伪品（包括鸭、鹅和鸽子的肌胃内膜）的方法。将超高效液相色谱-四极杆-静电场轨道阱质谱联用（UPLC-Q-Exactive Orbitrap-MS）与多元统计分析相结合，分析鸡内金及其掺伪品中的肽。通过pNovo结合手动光谱识别鉴定肽的结构，并使用合成肽标准品进行验证。采用液相色谱-串联质谱（LC-MS/MS）优化鸡内金中特征肽LESY的样品预处理条件，包括提取程序、提取时间、提取溶剂和溶剂量。采用电喷雾电离正离子模式（ESI⁺）下的多反应监测（MRM），以m/z 511.24→269.11和511.24→243.13作为检测离子进行定性和定量分析。所建立的超高效液相色谱-串联质谱（UPLC-MS/MS）方法具有良好的特异性、稳定性和耐用性。16批鸡内金样品中LESY的含量范围为55.03至113.36 μg·g⁻¹。此外，建立了一种掺伪品中常见肽RDPVLVSR的定性检测方法，以m/z 471.28→785.45和471.28→670.41作为检测离子。本研究建立了一种简便、快速、准确的鸡内金及其掺伪品特征肽检测方法。该方法具有良好的特异性、稳定性和耐用性，为鸡内金及其他动物源中药的鉴别和质量控制提供了有价值的参考。
