雷公藤片中5种有效成分同时测定及其质量评价研究  

Simultaneous determination and quality evaluation of five effective components in Tripterygium tablets

作　　者：谷升盼 付淑军[1] MUSSA Ally 寻明金[1] 圣勇 何新[1] 

机构地区：[1]天津中医药大学中药学院,天津300193

出　　处：《天津中医药》2015年第1期38-41,共4页Tianjin Journal of Traditional Chinese Medicine

基　　金：国家重点基础研究发展计划(973计划)资助项目(2012CB724001);天津市自然科学基金重点项目(12JCZD-JC26100)

摘　　要：[目的]建立雷公藤片中雷公藤甲素、雷公藤红素、雷公藤内酯甲、雷公藤定碱和雷酚内酯5种成分的液相色谱串联质谱法的同时定量测定的方法。[方法]采用液相色谱质谱联用技术(LC-MS/MS)测定含量,使用Zorbax XDB-C18(2.1 mm×50 mm,3.5μm)色谱柱,流动相采用40 mmol/L甲酸铵水溶液和0.1%甲酸甲醇溶液梯度洗脱,采用正离子模式大气压化学电离源(APCI源)。检测成分的离子对质荷比分别为:雷公藤甲素(361.0/105.0)、雷公藤红素(451.2/201.0)、雷公藤内酯甲(455.3/409.7)、雷公藤定碱(884.4/856.5)、雷酚内酯(313.2/225.2)。[结果]雷公藤甲素、雷公藤红素、雷公藤内酯甲、雷公藤定碱和雷酚内酯的线性关系良好(r>0.999),加样回收率分别为105.67%、94.07%、101.90%、99.28%、101.92%,RSD分别为2.65%、5.17%、2.68%、2.65%、3.27%。[结论]本研究所建立的LC-MS/MS分析方法稳定可靠、简便易行,可用于雷公藤片中雷公藤甲素、雷公藤红素、雷公藤内酯甲、雷公藤定碱和雷酚内酯5种成分的同时定量分析,为雷公藤片的质量评价和质量控制奠定了基础。[Objective] To establish an LC-MS/MS method for simultaneous determination of five effective componentsof Tripterygium tablets which are： triptolide, celastrol, wilforlide A, wilfordine and triptophenolide. [Methods] The assay was performed on a Zorbax XDB-C18 column （2.1 mm×50 mm, 3.5 μm） and was eluted with a mobile phase which consisted of the methonal of 0. 1% formic acid and 40 mmol/L ammonium formate. Atmospheric pressure chemical ionization source with positive ionization mode as well as selected ion monitoring mode was used in the detection. Ion used for quantification was m/z：361.0/105.0,451.2/201.0,455.3/409.7,884.4/856.5, 313.2/225.2, respectively. [Results] There was a good linear relationship over the studied concentration for the five studied components （r〉0.999）. The recoveries were 105.67% ,94.07%, 101.90% ,99.28%, 101.92%, respectively. The RSD corresponded were 2.65%, 5.17%, 2.68%, 2.65%, 3.27%. [Conclusion] The LC-MS/MS method developed for simultaneous determination of the five effective components is simple and valid. It can be used for quality evaluation and quality control of Tripterygium tablets.

关 键 词：雷公藤片 含量测定 液相色谱串联质谱法 

分 类 号：R284.2[医药卫生—中药学]