超高效液相色谱-三重四极杆质谱法检测阿胶补血颗粒中的阿胶  

RRLC/QQQ-MS analysis of donkey-hide gelatin in Ejiao Buxue granula

作　　者：龙国友 李明华[2] 刘薇[2] 陆以云 程显隆[2] 魏锋[2] 马双成[2] 

机构地区：[1]贵州省安顺市食品药品检验所,安顺561000 [2]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2016年第5期826-829,共4页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金青年项目"基于特征多肽识别技术和活性评价的龟甲胶与鹿角胶质量评价模式研究"(81202909);重大新药创制"中药安全检测技术及标准平台"(2014ZX09304307-002)

摘　　要：目的:建立阿胶补血颗粒中阿胶的专属性检测方法。方法:采用胰蛋白酶对阿胶补血颗粒中阿胶进行酶解,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。色谱柱为Agilent SB-C_(18)(2.1 mm×100 mm,1.8μm),流动相为0.1%甲酸溶液(A)-乙腈(B),梯度洗脱(0～25 min,95%A→80%A;25～40 min,80%A→50%A),流速0.3 m L·min^(-1),柱温40℃,进样量5μL;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:3批市售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,可用于阿胶补血颗粒中阿胶的检测。Objective：To establish an analysis method for specificity identification of donkey-hide gelatin in Ejiao Buxue granula.Methods：Samples were dissolved by water containing 1% NH_4HCO_3 and digested by trypsin.Ultra-high performance liquid chromatography（UPLC）coupled to triple quadruple mass spectrometry（QQQ MS）was used to detected the specific marker peptides in donkey-hide gelatins.Determination was carried out with the application of an Agilent SB-C_（18）（2.1 mm×100 mm,1.8 μm）column at temperature of 40 ℃.The mobile phase was composed of water solvent containing 0.1% formic acid（A）and acetonitrile（B）with gradient elution（0-25 min,95%A → 80%A;25-40 min,80%A → 50%A）at a flow rate of 0.3 m L·min_（-1）.The electrospray ionization（ESI）source was performed in multiple reaction monitoring（MRM）mode of the transitions of m/z 539.8（double charge）→ 612.4,m/z 539.8（double charge）→ 923.8.Results：The marker peptides can be detected in all samples by this method.Conclusion：The established method is specific,which is suitable for identification of donkey-hide gelatin in Ejiao Buxue granula.

关 键 词：阿胶补血颗粒 胰蛋白酶 酶解 特征肽段 阿胶检测 专属性鉴别 UPLC-QQQ MS 

分 类 号：R917[医药卫生—药物分析学]