高效液相色谱-三重四极杆质谱法检测暖宫孕子丸中阿胶特征肽成分  

Identification of donkey-hide gelatin in Nuangong Yunzi pills by UPLC-QQQ MS

作　　者：李广华 龙萍[2] 尹雪 程显隆[4] 魏锋[4] 马双成[4] LI Guang-hua;LONG Ping;YIN Xue;CHENG Xian-long;WEI Feng;MA Shuang-cheng(Liaocheng Food and Drug Inspection and Testing Center,Liaocheng 252000,China;Zibo Vocational Institue,Zibo 255314,China;Shandong Province Institute for Food and Drug Control,Jinan 250101,China;National Institutes for Food and Durg Control,Beijing 100050,China)

机构地区：[1]聊城市食品药品检验检测中心,聊城252000 [2]淄博职业学院,淄博255314 [3]山东省食品药品检验研究院,济南250101 [4]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2020年第4期694-697,共4页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金面上项目“基于特征肽段智能识别的鹿茸及相关产品真伪鉴别系统研究”(81773856);国家中药标准化项目“阿胶标准化”(ZYBZH-Y-SD-31)。

摘　　要：目的:建立暖宫孕子丸中阿胶特征肽成分的专属性检测方法。方法:采用胰蛋白酶对暖宫孕子丸样品进行酶解,利用超高效液相色谱-三重四极杆质谱(UPLC-QQQ MS)对阿胶的专属性特征肽段进行检测。采用Agilent SB-C18(2.1 mm×100 mm,1.8μm),以0.1%甲酸乙腈溶液(A)-0.1%甲酸水溶液(B)为流动相,梯度洗脱,流速0.3 mL·min^-1,柱温40℃;离子化模式为ESI^+,进行多反应监测,选择阿胶特征分子离子峰m/z 539.8(双电荷)→612.4,m/z 539.8(双电荷)→923.8作为检测离子对。结果:10批市售暖宫孕子丸样品中均可检出阿胶的特征肽段。结论:所建立的方法经方法学验证,专属性强,可用于暖宫孕子丸中阿胶的检测。Objective:To establish an analysis method for identification of donkey-hide gelatin in Nuangong Yunzi pills.Methods:Samples were dissolved by water containing 1%NH4HCO3 and digested by trypsin.Ultrahigh performance liquid chromatography(UPLC)coupled with triple quadruple mass spectrometry(QQQ MS)was used to detected marker peptide in donkey-hide gelatin.Determination was carried out on an Agilent SB-C18(2.1 mm×100 mm,1.8μm)column with the column temperature of 40℃.The mobile phase was composed of acetonitrile containing 0.1% formic acid(A)and 0.1% formic acid(B)with gradient elution at a flow rate of 0.3 mL·min^-1.The positive electrospray ionization(ESI^+)source was performed in multiple reaction monitoring(MRM)mode with the transitions of m/z 539.8(double charge)→612.4 and m/z 539.8(double charge)→923.8.Results:The marker peptides could be detected in all samples by this method.Conclusion:The established method is specific,which is suitable for identification of donkey-hide gelatin in Nuangong Yunzi pills.

关 键 词：暖宫孕子丸 阿胶 特征肽段 鉴别研究 标准提高 超高效液相色谱-三重四极杆质谱 

分 类 号：R917[医药卫生—药物分析学]