UPLC-MS/MS法快速测定降脂宁颗粒中4种化合物的含量

Rapid determination of four components in Jiangzhininggranules by UPLC-MS/MS

建立采用超高效液相色谱-串联质谱联用仪(ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时快速高效测定降脂宁颗粒中的金丝桃苷、二苯乙烯苷、荷叶碱、橙黄决明素含量的方法.采用Agilent Eclipse Plus C18(2.1 mm×50 mm,1.7μm)色谱柱;流动相是0.05%(体积分数)的甲酸水溶液和0.05%(体积分数)的甲酸-乙腈;流速0.3 mL/min;柱温40℃,进样量5μL;检测时间5 min.电喷雾(electrospray ionization,ESI)离子源,正离子扫描,多反应监测模式(multiple reaction monitoring,MRM).在所设的色谱条件下,5 min内能定量分析出降脂宁颗粒中4种成分,该4种化合物在考察范围内呈良好的线性关系(r≥0.993 6).精密度、稳定性和重复性考察符合分析要求,相对标准偏差(relative standard deviation,RSD)≤4.0%.加标回收率和RSD分别在98.0%~126.9%和0.3%~2.4%范围内.该分析方法简便、快速,灵敏度比较高,专属性强,能在5 min内同时测定降脂宁颗粒中的4种化合物含量,可以为降酯宁颗粒的生产与质量控制提供参考.

Developing a rapid and sensitive method for determining Hyperoside,Tetrahydroxystilbene glucoside,Nuciferine and Aurantio-obtusin in Jiangzhining granules with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The four components of Jiangzhining granules were separated into Agilent Eclipse Plus C 18 column(2.1 mm×50 mm,1.7μm)using 0.05%(volume fraction)formic acid-water(A)and 0.05%(volume fraction)formic acid-Acetonitrile(B)as the mobile phase with gradient elution.The flow rate was 0.3 mL/min and the column temperature was set at 40℃.The injection volume was 5μL,and analysis time was 5 min.The method we used is Electron Spray Ionization(ESI)with positive ion scanning and multiple reaction monitoring(MRM)mode for quantification.Under the optimized chromatographic conditions,four components of the Jiangzhining granules were quantitative analysis within 5 min,and showed a good linear relationship in the range of the study(r≥ 0.9936).It is worth noting that the RSDs of precision,stability and repeatability tests were all no more than 4.0%.The recoveries of four components ranged from 98.0%to 126.9%and RSDs were between 0.3%-2.4%.This method was simple,rapid,specific and accurate within 5 min for the determination of four components in Jiangzhining granules.The current method can be used for the quality control of Jiangzhining granules.