UPLC-MS/MS法同时测定静灵口服液中8种有效成分的含量  

Simultaneous determination of eight active ingredients in Jingling oral liquid by UPLC-MS/MS

作　　者：符丽 王雅溶 邹振庄 黄波 范庆 崔国祯 刘碧连 罗威 Fu Li;Wang Yarong;Zou Zhenzhuang;Huang Bo;Fan Qing;Cui Guozhen;Liu Bilian;Luo Wei(Zhuhai Ansheng Phoenix Pharmaceutical Co.,Ltd,Zhuhai Guangdong 519080,China;School of Bioengineering,Zhuhai Campus of Zunyi Medical University,Zhuhai Guangdong 519041,China;Pharmacy Intravenous Admixture Services,The Fifth Affiliated Hospital of Zunyi Medical University,Zhuhai Guangdong 519180,China)

机构地区：[1]珠海安生凤凰制药有限公司,广东珠海519080 [2]遵义医科大学珠海校区生物工程学院,广东珠海519041 [3]遵义医科大学第五附属(珠海)医院静配中心,广东珠海519180

出　　处：《遵义医科大学学报》2023年第12期1204-1210,共7页Journal of Zunyi Medical University

基　　金：遵义医科大学博士启动基金资助项目(NO:F-ZH-012)。

摘　　要：目的建立液相色谱-串联质谱法同时测定静灵口服液中盐酸小檗碱、远志口山酮Ⅲ、3,6′-二芥子酰基蔗糖、盐酸黄柏碱、芒果苷、细叶远志皂苷、五味子醇甲和特女贞苷8种主要成分的1/4含量。方法采用BEH C 18色谱柱(2.1×50 mm,1.7μm),流动相A为乙腈,流动相B为0.1%甲酸水溶液,柱温40℃,流速0.3 mL/min,梯度洗脱。质谱条件为电喷雾(ESI)离子源,正、负离子多反应离子监测(MRM)用于定量分析。结果盐酸小檗碱、远志口山酮Ⅲ、3,6′-二芥子酰基蔗糖、盐酸黄柏碱、芒果苷、细叶远志皂苷、五味子醇甲和特女贞苷分别在0.05~10、0.02~1、0.02~1、0.02~1、0.001~1、0.01~1、0.02~1、0.02~1μg/mL线性关系良好,平均加样回收率在98.4%~103.2%范围内,RSD≤4.34%。6批样品中上述8种成分的含量依次为22.39~29.43、2.75~8.85、7.58~9.58、10.08~20.11、0.09~0.61、9.31~11.71、0.55~5.39、6.45~28.08μg/mL。结论该方法操作简单、分离效果好、灵敏度高,具有良好的重复性和准确性,可以为静灵口服液的质量控制提供重要参考。Objective To establish an LC-MS/MS method for simultaneous quantification of 8 active ingredients(berberine hydrochloride,polygalaxanthone III,3,6′-disinapoyl sucrose,phellodendrine chloride,mangiferin,tenuifolin,schisandrin,nuezhenide)in Jingling oral liquid.Methods The chromatographic separation was performed on a BEH C 18 column(2.1×50 mm,1.7μm).During the gradient elution peroid,the mobile phase consisted of acetonitrile(A)and 0.1%formic acid(B)at a flow rate of 0.3 ml/min.The column temperature was controlled at 40℃.Positive and negative ion monitoring was carried out using electrospray ionization(ESI),and multiple reaction monitoring(MRM)was used for quantitative analysis.Results In this method,berberine hydrochloride,polygalaxanthone III,3,6′-disinapoyl sucrose,phellodendrine chloride,mangiferin,tenuifolin,schisandrin,and nuezhenide had good linear relationship between 0.05-10,0.02-1,0.02-1,0.02-1,0.001-1,0.01-1,0.02-1,and 0.02-1μg/ml respectively.The average recovery rates of 8 components were 98.4%-103.2%with RSDs less than 4.34%.The contents of 8 active components in 6 batches of Jingling oral liquid were 22.39-29.43,2.75-8.85,7.58-9.58,10.08-20.11,0.09-0.61,9.31-11.71,0.55-5.39,and 6.45-28.08μg/ml,respectively.Conclusion This method has the advantages of being simple to operate,having good separation effect and high sensitivity.It has been verified to have good repeatability and accuracy and can provide important reference for the quality control of Jingling oral liquid.

关 键 词：静灵口服液 质量控制 液质联用 含量测定 

分 类 号：R917[医药卫生—药物分析学]