HPLC-MS/MS同时测定心脑静片中5个生物碱类成分的含量  

Simultaneous determination of 5 alkaloids in Xinnaojingtablets by HPLC-MS/MS

作　　者：何风艳[1] 郭日新 武营雪 张海鸣[2] 戴忠[1] HE Feng-yan;GUO Ri-xin;WU Ying-xue;ZHANG Hai-ming;DAI Zhong(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7期1156-1162,共7页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立HPLC-MS/MS同时测定心脑静片中黄柏碱、异去氢钩藤碱、去氢钩藤碱、异钩藤碱和钩藤碱5个生物碱类成分含量的方法。方法:采用Waters Acquity UPLC BEH C18色谱柱(50 mm×2.1 mm, 1.7μm),以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,流速为0.4 mL·min^(–1);质谱采用正离子扫描,多反应监测(MRM)模式进行定量分析。结果:5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>0.999 5;平均回收率(n=6)在93.4%~104.0%,RSD在1.2%~3.2%。2个厂家14批样品中黄柏碱、异去氢钩藤碱、去氢钩藤碱、异钩藤碱和钩藤碱的含量分别为218.08~716.22、3.24~64.47、6.65~207.74、1.47~39.68、3.87~98.89μg·g^(-1)。不同厂家样品中黄柏碱的测定结果较为接近,而异去氢钩藤碱、去氢钩藤碱、异钩藤碱、钩藤碱的含量测定结果差异较大。结论:本方法灵敏、准确,可用于心脑静片相关药味的质量控制。Objective:To establish an HPLC-MS/MS method for simultaneous determination of 5 alkaloids(phellodendrine,isocorynoxeine,corynoxeine,isorhynchophylline,and rhynchophylline)in Xinnaojing tablets.Methods:HPLC assay was performed on Waters Acquity UPLC BEH Cis column(50 mm×2.1 mm,1.7μm)with a mixture of acetonitrile and 0.1%formic acid as the mobile phase in gradient elution at a flow rate of 0.4 mL·min^(-1).Detection was carried out on a triple quadrupole mass spectrometer in positive ion mode using an electrospray source.Multiple reaction monitoring(MRM)mode was employed.Results:All 5 components showed good linearity(r>0.9995).The average recoveries(n=6)were in the range of 93.4%-104.0%with RSD in the range of 1.2%-3.2%.The contents of phellodendrine,isocorynoxeine,corynoxeine,isorhynchophylline,and rhynchophylline in 14 tested samples from 2 manufacturers were 218.08-716.22μg·g^(-1),3.24-64.47μg·g^(-1),6.65-207.74μg·g^(-1),1.47-39.68μg·g^(-1),and 3.87-98.89μg·g^(-1).Except for phellodendrine,the tested alkaloids in samples from different manufacturers varied significantly.Conclusion:The developed method is accurate and sensitive.It can be used in quality control of related herbs in Xinnaojing tablets.

关 键 词：心脑静片 黄柏碱 异去氢钩藤碱 去氢钩藤碱 异钩藤碱 钩藤碱 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]