超高效液相色谱-质谱法检测妇科止带胶囊中马皮源成分

UPLC-MS Analysis of Equine-hide Gelatin in Fuke Zhidai Capsules

目的:建立妇科止带胶囊中可能掺杂的马皮源成分的测定方法。方法:以马皮中的专属性特征肽段为检测指标,对样品进行恒温酶切处理,采用超高效液相色谱-串联质谱技术进行识别。ESI正离子化模式,以马皮源的特征离子对进行检测,多反应监测。结果:经方法学验证,马源寡肽A对照品在0.03638~0.7276μg/mL范围内线性关系良好(r=0.9978),建立的限量检查方法专属性强、重复性佳、稳定性好。用建立的方法测定妇科止带胶囊样品,均未发现马皮源成分。结论:该检测方法灵敏度高、专属性强、准确快速,为妇科止带胶囊中马皮源成分的检测提供了参考。

Objective:A method for the determination of equine-hide gelatin possibly doped in fuke zhidai capsules was established.Methods:The exclusive characteristic peptides in equine were used as the detection index.The characteristic peptides contained in the samples were digested at constant temperature and identified by UPLC-MS.ESI(+)ionization mode,with the characteristic ion pair of equine-hide gelatin for detection and multi reaction monitoring were adopted.Results:The linear relationship of peptide A equine was good in the range of 0.03638-0.7276μg/mL with the correlation coefficient of 0.9978.According to the verification of methodology,this method had strong specificity,stability and repeatability.Equine-hide gelatin was not detected in 8 batches samples.Conclusion:The method has the advantages of high sensitivity,strong specificity,accuracy and rapidity,and provides a reference for the detection of equine-hide gelatin in fuke zhidai capsules.