摘要
目的建立液相色谱-串联质谱(LC-MS/MS)分析方法,以同时分离测定复方救必应胶囊中3种互为同分异构体的有效成分(α-香附酮、香附烯酮、圆柚酮),并对随机抽样的3批复方救必应胶囊进行质量分数比较。方法采用Simpsil C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.1%甲酸水溶液(体积比95∶5)为流动相,25 min内进行等度洗脱。流速为0.3 mL/min,柱温为室温,进样量为20.0μL。选用电喷雾离子源(ESI),正离子模式下多反应监测扫描(MRM),优化相关质谱参数,对3种有效成分进行检测和定量分析。结果α-香附酮、香附烯酮在质量浓度0.45～200μg/L范围内线性关系良好(r≥0.996 6);圆柚酮在质量浓度3～1 500μg/L范围内线性关系良好(r=0.996 0)。α-香附酮、香附烯酮、圆柚酮的平均加样回收率皆在95%～105%,RSD<3.5%(n=6)。3批复方救必应胶囊中α-香附酮、香附烯酮、圆柚酮的平均质量分数分别为437.17、847.39、42.92μg/g,RSD<15%。结论本方法准确可靠、结果稳定、重复性良好、灵敏度高,可用于复方救必应胶囊中3种同分异构体有效成分的质量分数测定。
Objective To establish an LC-MS method for the simultaneous determination of the three effective components(α-cyperone,cyperotundone and nootkatone)in compound Jiubiying capsules,and to compare the mass fractions of three batches of compound Jiubiying capsules sampled randomly.Methods A Simpsil C18column(250mm×4.6mm,5μm)was used with a mobile phase containing acetonitrile and0.5%formic acid water(95∶5),the separation was carried out in isocratic mode within25minutes.The flow rate was0.3mL/min,the column temperature was room temperature,and the injection volume was20.0μL.The electrospray ionization source(ESI)was used to perform multi-reaction monitoring scanning(MRM)in positive ion mode,and the relevant mass spectrometry parameters were optimized to detect and quantify the three active components.Resultsα-cyperone and cyperotundone had a good linear relationship(r≥0.9966)in the concentration range of0.45-200μg/L,and the linear relationship of nootkatone was good(r=0.9960)in the concentration range of3-1500μg/L.The average recovery(n=6)ofα-cyperone,cyperotundone and nootkatone was between95%and105%,RSD<3.5%.The average content ofα-cyperone,cyperotundone,and nootkatone in three batches of compound Jiubiying capsules was437.17,847.39,42.92μg/g,RSD<15%.Conclusion The method is accurate,reliable,stable,reproducible and sensitive,which can be used to determine the content of three isomers in compound Jiubiying capsules.
作者
黄明萍
谢水林
戴仁科
HUANG Mingping;XIE Shuilin;DAI Renke(Biology and Biological Engineering School,South China University of Technology,Guangzhou 510006,China;ZhongShan Pharmass Corporation,Zhongshan 528400,China)
出处
《广东药科大学学报》
CAS
2018年第6期695-699,708,共6页
Journal of Guangdong Pharmaceutical University
基金
广东省高新区发展引导专项计划(2012B011000039)
广东省科技计划项目(2013A022100019)
