液相色谱-串联质谱法同时测定地榆槐角丸中9种化学成分  

Simultaneous determination of nine constituents in Di-Yu-Huai-Jiao pill by LC-MS/MS

作　　者：靳怡然[1,2] 田婷婷[1] 贺璠 马英华[1] 许慧君[1] 杜英峰[1] 

机构地区：[1]河北医科大学药学院药物分析学教研室,河北石家庄050017 [2]河北医科大学第二医院药学部,河北石家庄050000

出　　处：《河北医科大学学报》2015年第7期745-749,共5页Journal of Hebei Medical University

基　　金：国家自然科学资金项目(81402894)

摘　　要：目的建立液相色谱-串联质谱法同时测定地榆槐角丸中芦丁、槐角苷、柚皮苷、染料木苷、黄芩苷、染料木素、芦荟大黄素、大黄酸和大黄素含量的方法。方法采用C18色谱柱,乙腈-0.1%乙酸水为流动相,梯度洗脱。采用电喷雾离子源,监测模式为负离子,定量检测采用多重反应离子模式。结果在15min内地榆槐角丸中9种有效成分在所测定的浓度范围内线性关系均良好,加样回收率(n=3)分别为96.2%、97.5%、98.3%、99.6%、97.5%、100.1%、94.2%、98.7%和99.7%,相对标准偏差(relative standard deviation,RSD)值分别为1.3%、1.2%、1.4%、1.7%、0.5%、0.54%、0.9%、1.0%和0.82%。结论该方法简便、准确、重现性好、专属性高,可用于地榆槐角丸的质量控制。Objective To develop a method for the simultaneous determination of rutin,sophoricoside,naringin,genistin,baicalin,genistein,aloe-emodin,rhein and emodin in Di-Yu-HuaiJiao pill.Methods C18 column was used with the mobile phase of acetonitrile 0.1% aqueous acetic acid water with gradient elution.The identification and quantification of the analytes were achieved on multiple-reaction monitoring scanning（MRM）under negative ion scanning mode with electrospray ionization（ESI）.Results There were significant correlation between the ratio of peak area and the concentration of each compound within the test ranges.The average recoveries（n=3）of the nine compounds listed above were 96.2%,97.5%,98.3%,99.6%,97.5%,100.1%,94.2%,98.7% and 99.7%.The RSDs were 1.3%,1.2%,1.4%,1.7%,0.5%,0.54%,0.9%,1.0% and 0.8%,respectively.Conclusion The method is simple,accurate and highly reproducible,and can be used for the determination of nine compounds in Di-Yu-Huai-Jiao pill.

关 键 词：地榆槐角丸 色谱法 液相 串联质谱法 含量测定 

分 类 号：R972.6[医药卫生—药品]