超高效液相色谱-质谱联用技术检测阿胶中马皮源成分

目的：建立阿胶中马皮源成分的检测方法，为阿胶药材质量控制提供技术支持。方法：利用高分辨质谱分析方法获得马皮中专属特征肽段，采用胰蛋白酶对阿胶进行酶解，经超高效液相色谱-三重四极杆质谱对马源寡肽段进行检测。电喷雾离子化（ESI），正离子模式下，进行多反应监测，选择马皮特征分子离子峰m/z 386.4（双电荷）→377.3，322.3作为检测离子对。结果：方法学试验考察表明，所建立方法专属性、稳定性、重复性及耐用性均良好，对照物质马源寡肽A线性范围为0.010 86~1.086 μg·mL^-1，相关系数为0.999 9。以所建立的方法对专项抽验的56批阿胶进行检验，结果28批样品检出马皮源成分。结论：所建立的方法准确可靠，专属性强，可用于阿胶中的马皮源成分的检测。

Objective:To establish an analysis method for specific identification of equine-hide gelatin in Ejiao.Method:The UPLC-MS was used to find the marker peptides for identification of equine-hide gelatin in Ejiao.The sample was analyzed on UPLC coupled with triple quadrupole mass spectrometry after digesting by trypsin.Choosing the characteristic molecular peaks of m/z 386.4→377.3, 322.3 as target ion pair, collagen marker peptides were detected by mass spectrometry with positive electrospray ionization and multiple reaction monitoring (MRM).Results:The methodological evaluation showed that this method had good specificity, stability, repeatability and durability.The linear ranges of peptide A equine fell within the ranges of 0.010 86-1.086 μg·mL^-1 with the correlation coefficient of 0.999 9.The characteristic molecular peaks of equine-hide gelatin were detected in 28 batches of Ejiao.Conclusion:The present method is specific, precise, reliable, and suitable for identification of equine-hide gelatin in Ejiao.

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