HPLC-MS/MS法同时测定心脑静片中10个成分的含量  

Simultaneous determination of 10 components in Xinnaojingg tablets by HPLC-MS/MS

作　　者：何风艳[1] 周亚楠 戴忠[1] 张海鸣[2] 马双成[1] HE Feng-yan;ZHOU Ya-nan;DAI Zhong;ZHANG Hai-ming;MA Shuang-cheng(National Institutes for Food and Drug Control,Beijing 100050,China;Experimental Research Center,China Academy of Chinese Medical Sciences,Beijing 100700,China)

机构地区：[1]中国食品药品检定研究院,北京100050 [2]中国中医科学院医学实验中心,北京100700

出　　处：《药物分析杂志》2023年第4期564-572,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药品标准制修订研究课题(2021Z15)。

摘　　要：目的:建立HPLC-MS/MS同时测定心脑静片中10个成分含量的方法。方法:采用Agilent Zorbax Eclipse Plus C_(18)(50mm×2.1mm,1.8μm)色谱柱,以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,流速为0.4mL·min^(-1),柱温为30℃,进样量为1μL;质谱采用负离子扫描,多反应监测(MRM)模式进行定量分析。结果:10个成分在一定浓度范围内与峰面积呈良好线性关系,线性相关系数r均>0.9990;平均回收率(n=6)在94.9%~107.9%,RSD在0.9%~3.4%。2个厂家14批样品中绿原酸、龙胆苦苷、甘草苷、甘草酸、芦丁、迷迭香酸、汉黄芩苷、黄芩素、汉黄芩素、喜果苷的含量分别为0.49~1.24、1.75~4.14、0.06~0.13、0.19~0.48、24.53~35.55、0.56~1.17、6.31~10.22、0.96~2.89、0.48~1.28、0.03~0.08mg·g^(-1)。除喜果苷外,不同厂家样品中其他9个成分的测定结果较为接近。结论:本方法灵敏、准确,可用于心脑静片的质量控制。Objective:To establish an HPLC-MS/MS method for simultaneous determination of 10 components in Xinnaojing tablets.Methods:HPLC assay was performed on Agilent Zorbax Eclipse Plus C_(18)(50 mm×2.1 mm,1.8μm)column with a mixture of acetonitrile and 0.1%formic acid as the mobile phase in gradient elution at a flow rate of O.4 mL·min^(-1).The column temperature was 30℃and the injection volume was 1μL.Detection was carried out on a triple quadrupole mass spectrometer in negative ion mode using an electrospray source.Multiple reaction monitoring(MRM)mode was employed.Results:All 10 components showed good linearity(r>0.9990).The average recoveries(n=6)were in the range of 94.9%-107.9%with RSDs within 0.9%-3.4%.The contents of chlorogenic acid,gentiopicrin,liquiritin,glycyrrhizic acid,rutoside,rosmarinic acid,wogonoside,baicalein,wogonin and vincosamide in 14 tested samples from 2 manufacturers were 0.49-1.24,1.75-4.14,0.06-0.13,0.19-0.48,24.53-35.55,0.56-1.17,6.31-10.22,0.96-2.89,0.48-1.28,and 0.03-0.08 mg·g^(-1).Except for vincosamide,the contents of other 9 investigated components in tested samples from different manufacturers were close.Conclusion:The developed method is accurate and sensitive.It can be used in quality control of Xinnaojing tablets.

关 键 词：心脑静片 绿原酸 龙胆苦苷 甘草苷 甘草酸 芦丁 迷迭香酸 汉黄芩苷 黄芩素 汉黄芩素 喜果苷 中成药质量控制 高效液相色谱-串联质谱法 

分 类 号：R917[医药卫生—药物分析学]