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.
出处
《天津中医药》
CAS
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)
