基于UPLC-MS/MS技术测定药材中川楝素的方法研究  

Determination of Toosendanin in Medicinal Herbs Based on UPLC-MS/MS Technique

作　　者：李智宁[1] 范毅[1] 李自红[1] 李飞飞[1] 宋梦娇 曹静亚[1] 张丽先[1] 宁二娟 魏悦[1] 

机构地区：[1]河南省生物技术开发中心,郑州450002

出　　处：《河南科学》2017年第9期1406-1411,共6页Henan Science

基　　金：河南省科技攻关项目(162102310345)

摘　　要：为了建立并验证一个液相色谱串联三重四级杆质谱法(LC-MS/MS)测定药材中的川楝素,供试品经甲醇水浴回流提取后,采用Agilent Eclipse Plus C18色谱柱(4.6 mm×100 mm,3.5μm),以乙腈-0.01%甲酸水溶液为流动相梯度洗脱,流速为0.5 mL/min,柱温30℃,进样量2μL.质谱条件为电喷雾电离源(ESI),负离子模式,选择离子监测(SIM),用于定量的离子为573.1.结果显示,川楝素在42.73~2 136.40 ng/mL范围内线性关系良好(R2=0.999 6),加样回收率为99.34%~106.53%,日内、日间精密度(RSD)均低于3%,最低检出限(LOD)为0.92 mg/kg,最低定量限(LOQ)为3.05 mg/kg,稳定性较好.说明所建方法能够高效快捷地对川楝素进行测定,且方法简便、专属性强、灵敏度高,测定结果准确可靠,适用于川楝子、苦楝皮中川楝素的定性定量测定,也为其新制剂的设计和开发提供方法参考.A method for the determination of toosendanin in medicinal herbs was established and validated by ultrahigh pressure liquid chromatography-tandem quadrupole mass spectrometry（UPLC-MS/MS）. The purified samplewas extracted with methanol under reflux in water bath and eluted with Agilent Eclipse Plus C18 column（RRHD3.5 μm,4.6 mm×100 mm）and eluting with acetonitrile-0.01% formic acid as the mobile phase gradient at a flow rateof 0.5 mL/min,and the column temperature 30 ℃,and the injection volume was 2 μL. The mass spectrometricconditions were electrospray ionization（ESI）,negative ion mode,Detection was carried out by select ion monitoringmode（SIM）of the transitions（precursor ion）at m/z 573.1 for toosendanin. The linear range was 42.73-2 136.40 ng/m L,the recoveries were 99.34%-06.53%,and all the RSD of intra and inter-day precisions were less than 3%（n=3）,the limit of detection（LOD）of toosendanin was 0.92 mg/kg and the limit of quantification（LOQ）was 3.05 mg/kg.The stability was better. It was shown that the method could be used for the determination of toosendanin efficientlyand rapidly. The method is of sample operation,strong specificity,high sensitivity and the measured results areaccurate and reliable. It can be used for the qualitative and quantitative determination of toosendanin in toosendanand melia azedarach and to provide a method reference for the design and development of the new formulations.

关 键 词：川楝素 UPLC-MS/MS 川楝子 苦楝皮 

分 类 号：R282.5[医药卫生—中药学]