HPLC-MS/MS法同时测定肿节风中8种化学成分含量

Simultaneous Determination of Eight Effective Components in Sarcandra Glabra by HPLC-MS/MS

目的:采用HPLC-MS/MS同时测定肿节风中的刺五加苷b1、咖啡酸、芦丁、迷迭香酸、绿原酸、隐绿原酸、新绿原酸和异嗪皮啶等8种化学成分含量。方法:采用Waters ACQUITY UPLC?BEH C18色谱柱(2.1 mm×100 mm,1.7μm);以乙腈-水(含0.04%的甲酸)为流动相,梯度洗脱,流速为0.25 mL/min,进样量5μL,柱温35℃;电喷雾离子化源(ESI);多反应监测模式(MRM)进行定性定量分析。结果:在该色谱条件下,肿节风中8种化学成分在各自范围内,峰面积和浓度呈良好的线性关系(r>0.995),平均加样回收率(n=9)为97.85%~102.89%,RSD为0.89~2.36,经过测定6个产地的肿节风中刺五加苷b1、咖啡酸、芦丁、迷迭香酸、绿原酸、隐绿原酸、新绿原酸、异嗪皮啶的含量依次为4.9~40.8μg/g、642.7~1096.5μg/g、5.4~100.6μg/g、908.8~2488.9μg/g、138.8~975.2μg/g、90.9~506.1μg/g、89.6~707.4μg/g、986.1~1840.8μg/g。结论:该方法准确,重现性好,专属性高,可用于肿节风的质量控制。

Objective:To develop a HPLC-MS/MS method for determining in Sarcandra glabra.Methods:Analysis was performed on a Waters ACQUITY UPLC BEH C 18 column(2.1 mm×100 mm,1.7μm)with a gradient elution of acetonitile and water containing 0.04%formic acid at a 0.25 mL/min flow rate.The injection volume was 5μL,and the column temperature was controlled at 35℃.The multiple-reaction monitoring scanning was employed for the quantification with switching electrospray ion source polarity in negative mode.Results:There was a significant correlation between each compound's peak area and concentration within the test range(r>0.995).The average recoveries(n=9)of the compounds ranged from 97.85%to 102.89%.The contents of Eleutheroside b1,Caffeic acid,Rutin,Rosmarinic acid,Chlorogenic acid,Cryptochlorogenic acid,Neochlorogenic acid,Isofraxidin in 6 batches of Sarcandrae Herba were 4.9-40.8μg/g,642.7-1096.5μg/g,5.4-100.6μg/g,908.8-2488.9μg/g,138.8-975.2μg/g,90.9-506.1μg/g,89.6-707.4μg/g,986.1-1840.8μg/g.Conclusion:The established method is simple,accurate and highly reproducible,which can be used for quality control of Sarcandra glabra.