超高效液相色谱-质谱联用技术评价当归养血丸中阿胶投料情况

Quality Evaluation of Ass-hide Gelatin in Danggui Yangxue Pill by UPLC-MS

目的建立当归养血丸中阿胶的检测方法,为投料阿胶质量控制提供技术支持。方法采用胰蛋白酶对当归养血丸进行酶解,利用超高效液相色谱-质谱联用技术(UPLC-MS/MS),在电喷雾离子化(ESI+)模式下,进行多反应监测(multiple reaction monitoring,MRM),进行阿胶专属鉴别、马皮源成分检查及阿胶特征多肽含量测定。结果建立方法线性、专属性、稳定性、重复性、耐用性良好。以此方法,11批当归养血丸中均检出阿胶,其中9批检出马皮源成分,7批低于阿胶特征多肽含量拟定限度。结论所建立的方法准确可靠、专属性强,可用于当归养血丸中阿胶的质量评价。

OBJECTIVE To establish an analysis method for specific identification of ass-hide gelatin in Danggui Yangxue Pill.METHODS The UPLC-MS/MS was used to establish the identification of ass-hide gelatin、equine-hide gelatin and content determination of marker peptides for Danggui Yangxue Pill.The sample was analyzed on UPLC coupled with triple quadrupole mass spectrometry after digesting by trypsin.Choosing the characteristic molecular peaks 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 linearity,specificity,stability,repeatability and durability.Ass-hide gelatin was detected out in 11 batches of samples,while equine-hide gelatin was detected in 9 batches and 7 batches below the content limit.The series methods established in this paper provide technical support for the evaluation of the Chinese medicine preparations containing ass-hide gelatin.CONCLUSION The present method is specific,precise,reliable,and suitable for quality evaluation of ass-hide gelatin in Danggui Yangxue Pill.