超高效液相色谱-三重四极杆质谱法检测补血益母丸中阿胶  

Qualitative UPLC-QQQ/MS analysis of donkey-hide gelatin in Buxue Yimu pills

作　　者：陈鸿玉[1,2] 李文莉[1,2] 李劲平[1] 杨青 李玲[1] 童达 高洁莹 

机构地区：[1]中南大学药学院,长沙410013 [2]湖南省药品检验研究院,长沙410001

出　　处：《中南药学》2016年第5期540-543,共4页Central South Pharmacy

基　　金：湖南省食品药品监督管理局食品药品安全科技项目"含阿胶中成药中阿胶的检测方法研究"(湘食药科R201504);国家科技重大专项课题(编号:2014ZX09304307-002)

摘　　要：目的建立补血益母丸中阿胶的专属性检测方法。方法采用胰蛋白酶对补血益母丸中阿胶成分进行酶解,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分子离子峰进行检测。采用Hypersil GOLD C18(2.1 mm×75 mm,3.0μm)色谱柱,以0.1%甲酸水溶液-乙腈系统梯度洗脱,流速0.3 m L·min-1,柱温30℃,进样量5μL;选择阿胶特征分子离子峰m/z 539.8(双电荷)→612.4和m/z 539.8(双电荷)→923.8作为检测离子对,离子化模式为ESI+,进行多反应监测。结果20批市售样品中均可检出阿胶的特征分子离子峰,即同时检出m/z 539.8(双电荷)→612.4和m/z539.8(双电荷)→923.8离子对。结论所建立的方法经方法学验证,阴性样品及其他胶类如黄明胶(牛皮)、猪皮胶、鹿角胶对补血益母丸样品测定无干扰。方法专属性强,可用于补血益母丸中阿胶的检测。Objective To establish an analytical method to identify donkey-hide gelatin in Buxue Yimu pills. Methods Identification of donkey-hide gelatin in Buxue Yimu pills was established by rapid resolution liquid chromatography （UPLC） coupled to triple quadruple mass spectrometry （QQQ-MS）. Chromatographic separation was carried out on an Hypersil GOLD C18 reversed phase analytical column （75 mm ×2.1 mm, 3.0 μm） at a column temperature of 30℃ . The mobile phase consisted of 0.1% formic acid in water and acetonitrile in gradient mode at 0.3 mL · min-1, and the injection volume was 5 μL. Collagen marker peptides were detected by mass spectrometry in the positive electrospray ionization with multiple reaction monitoring. Results The characteristic molecular peaks of donkey-hide gelatin m/z 539.8 → 612.4 and m/z 539.8 → 923.8 were detected in all 20 batches of commercial samples. Conclusion Methodological verification shows that the donkey-hide gelatin does not interfere with the negative gelatins and other gelatins such as bovine-hide gelatin, pigskin gelatin and deer-horn glue. The present method is specific, precise and reliable, and is suitable for the identification of donkey-hide gelatin in Buxue Yimu pills.

关 键 词：超高效液相色谱-三重四极杆质谱 补血益母丸 阿胶 特征分子离子峰 

分 类 号：R917[医药卫生—药物分析学]