UHPLC-ESI-MS/MS同时测定尿毒康合剂中11种成分的含量

Simultaneous Determination of 11 Components in Niaodukang Mixture by UHPLC-ESI-MS/MS

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InertSustain^(R) C_(18)(3.0 mm×100 mm,3.0μm)色谱柱,甲醇(A)-0.1%甲酸水溶液(B),梯度洗脱,流速0.4 mL·min^(−1),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<3.0%,加样回收率为98.44%~103.56%,RSD为2.04%~3.34%。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依据。

OBJECTIVE To established a 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 in Niaodukang mixture.METHODS InertSustain^(R) C_(18)(3.0 mm×100 mm,3.0μm)column was used,mobile phase was methanol(A)-0.1%formic acid(B)with gradient elution at a flow rate of 0.4 mL·min^(−1),and the injection volume was 20μL.The mass spectrometry used the electrospray ionization source(ESI source).Multiple-reaction monitoring was employed with switching electrospray ion source polarity in positive and negative mode.RESULTS The peak area and mass concentration of 11 components in Niaodukang mixture showed a good linear relationship within the linear range.The precision of RSD were<3.0%,the average recoveries ranged from 98.44%to 103.56%,RSD ranged from 2.04%to 3.34%.CONCLUSION The method is stable,accurate,and simple,which can be used to control and evaluate the quality of Niaodukang mixture.It can also provide evidence for clinical application and research of Niaodukang mixture.