超高效液相色谱-三重四级杆串联质谱法同时测定增乳膏中6种成分  

Simultaneous determination of six components in Zengru Gao by UPLC-MS/MS

作　　者：黄淑芬 HUANG Shufen(Zhangzhou Pien Tze Huang Pharmaceutical Co.,Ltd.,Zhangzhou 363000,China)

机构地区：[1]漳州片仔癀药业股份有限公司,福建漳州363000

出　　处：《化学分析计量》2024年第9期22-27,共6页Chemical Analysis And Meterage

基　　金：中成药创新闽港科技合作基地项目(2021D045)。

摘　　要：建立超高效液相色谱-三重四级杆串联质谱法同时测定增乳膏中6种成分(盐酸水苏碱、王不留行黄酮苷、盐酸益母草碱、芍药苷、阿魏酸、毛蕊花糖苷)。样品经甲醇超声提取,采用Waters XBridge BEH C_(18)色谱柱分离,流动相为乙腈-0.1%甲酸水溶液,流量为0.3 mL/min,柱温为30℃,进样体积为2μL。采用电喷雾电离源(ESI源)、正负离子同时监测、多反应监测(MRM)模式扫描。6种成分在各自质量浓度范围内与对应色谱峰面积呈良好的线性关系,相关系数均不小于0.9998,方法检出限为0.035~0.535 ng/mL,定量限为0.100~1.605 ng/mL。样品加标平均回收率为98.08%~103.11%,测定结果的相对标准偏差为1.94%~3.67%(n=6)。该方法适用于同时测定增乳膏中6种成分的含量,可为增乳膏的质量标准修订提供参考。A method for simultaneous determination of 6 components(stachydrine hydrochloride,vaccarin,leonurine hydrochloride,paeoniflorin,ferulic acid and verbascoside)in Zengru Gao by ultra high performance liquid chromatography-triple quadrupole tandem mass spectrometry was established.The sample was ultrasonically extracted by methanol and separated using a Waters XBridge BEH C_(18) chromatographic column.The mobile phase was acetonitrile-0.1%formic acid aqueous solution,the flow rate was 0.3 mL/min,the column temperature was 30℃,and the injection volume was 2μL.Electrospray ionization source(ESI source),simultaneous monitoring of positive and negative ions,and multi reaction monitoring(MRM)mode scanning were used.The 6 components had a good linear relationship with corresponding chromatographic peak area in the respective mass concentration ranges,with correlation coefficients not less than 0.9998.The detection limits of the method were 0.035-0.535 ng/mL,and the quantitative limits were 0.100-1.605 ng/mL.The average recoveries were 98.08%-103.11%,and the relative standard deviations of the measurement results were 1.94%-3.67%(n=6).This method is suitable for simultaneously determining the content of 6 components in Zengru Gao,which provide reference for the revision of quality standards for Zengru Gao.

关 键 词：增乳膏 超高效液相色谱-串联质谱法 盐酸水苏碱 王不留行黄酮苷 盐酸益母草碱 芍药苷 阿魏酸 毛蕊花糖苷 

分 类 号：O657.7[理学—分析化学]