UPLC-QTOF-MS技术用于胶类药材的专属性检测方法研究应用.pdfVIP

UPLC-QTOF-MS技术用于胶类药材的专属性检测方法研究及应用∗ 魏锋，程显隆，石岩，肖新月，马双成，林瑞超 (中国食品药品检定研究院,北京 100050) 摘要 目的：针对胶类经材的主要成分及特点，利用液质联用法建立专属性的鉴别和检 测方法。方法：使用胰蛋白酶对龟甲胶、鹿角胶、阿胶、黄明胶、新阿胶等5种常用胶 类药材进行酶解，利用超高效液相色谱-四极杆-飞行时间质谱（UPLC-Q-TOF）进行测定， 再以PCA为引导，寻找具有专属性鉴别意义的特征肽段。结果：按照以上方法，分别找 出龟甲胶、鹿角胶、阿胶、黄明胶、新阿胶的特征肽段，对特征肽的氨基酸序列进行了 确认，并进行了方法学验证。结论：所建立的方法经过系统验证，重复性好，专属性强， 可用于5种常用胶类药材的专属性鉴别，并成功应用于相关产品的市场监督工作。 关键词：UPLC-QTOF-MS, 胶类药材, 特征肽段, 氨基酸序列，专属性检测, PCA Method development and application of UPLC-QTOF-MS for identification of five gelatin drugs * Feng Wei, Xian-Long Cheng, Yan Shi, Xin-Yue Xiao, Shuang-Cheng Ma, Rui-Chao Lin (National Institutes for Food and Drug Control, State Food and Drug Administration, Beijing, 100050) Abstract Objective:To develop an UPLC-Q-TOF method for Identification of donkey-hide gelatin, bovine-hide gelatin, pig-hide gelatin, glue of Tortoise shell, deerhorn glue. Methods: The sample was were digested by trypsin, the analysis of tryptic peptides was performed with a UPLC equipped with a TOF MS. PCA was performed on the UPLC MS data obtained from the peptides chromatography。 Results: The marker peptides were determined though the loadings plot of PCA, and were identified tentatively by the accurate mass of TOF/MS and partially verified by the Biopharmalynx 1.2. The marker peptides can be detected from the Glue of Tortoise Shell and Deer-horn Gelatin bought in the market. Conclusion: ∗[基金项目]：科技部重大专项“中药质量标准研究和信息化体系建设平台”(2009ZX09308-004) ；中国食品药品检定 研究院中青年发展研究基金（2010A1 ） Results from this study indicate that the proposed method is reliable for Identification of five commonly used Gelatin drugs in TCM, and the method was successfully applied in quality surveillance of Gelatin drugs in chinese market. Key words : UPLC-QTOF-MS, gelatin, polypeptide,