UHPLC-ESI-MS/MS测定尿毒康合剂中11种成分的含量

Simultaneous Determination of 11 Components in Niao-du-kang Mixture by UHPLC-ESI-MS/MS

关键词:  液质联用  尿毒康合剂  含量测定；多重反应监测

Key words:  UHPLC-ESI-MS/MS  Niao-du-kang Mixture  Content determination  MRM

摘要:

目的 建立UHPLC-ESI-MS/MS法同时测定尿毒康合剂中没食子酸、毛蕊异黄酮葡萄糖、芦丁、金丝桃苷、丹酚酸B、大黄酸、黄芪甲苷、隐丹参酮、大黄素、丹参酮I、丹参酮IIA的含量。方法 采用InertSustainC18 (3.0 mm×100 mm , 3.0 μm) 色谱柱，甲醇-0.1%甲酸水溶液，梯度洗脱，流速0.4mL/min，进样量20μL；质谱采用电喷雾离子源（ESI 源），正负离子扫描切换，多重反应监测模式进行定量分析。结果 尿毒康合剂中11种成分在线性范围内峰面积与质量浓度均呈良好的线性关系，仪器精密度RSD值小于3.0%，加样回收率为98.10%～104.17%，RSD为1.99%～3.26%。结论 本方法高效、稳定、准确、简便，可用于尿毒康合剂中的质量评价与质量控制，并为尿毒康合剂中的临床应用及研究提供科学依据。

Abstract:

OBJECTIVE To develop an UHPLC-ESI-MS/MS method for simultaneous determination of gallic acid, calycosin-7-glucoside, rutin, hyperoside, salvianolic acid B, rhein, astragaloside IV, cryptotanshinone, emodin, tanshinone I, tanshinone IIA. METHODS The separation was performed on a InertSustain C18 (3.0 mm×100 mm, 3.0 μm) column mobile phase consisting of water (containing 0.1% formic acid) and Methanol with gradient elution at a flow rate of 0.4 mL/min, and the injection volume was 20μL. Multiple-reaction monitoring (MRM) was employed with switching electrospray ion source polarity in positive and negative mode. RESULTS For the UHPLC-ESI-MS/MS assay, the calibration curve was linear, the precision of RSD were less than 3.0%, the average recoveries ranged from 98.10% to 104.17%，RSD ranged from 1.99% to 3.26%. CONCLUSION The established UHPLC-ESI-MS/MS method is simple, stable, rapid and correct, and can be used to control and evaluate the quality of Niao-du-kang Mixture; and can provide scientific basis for clinical application.